Category: 6443-69-2

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 6443-69-2, name is 1,2,3-Trimethoxy-5-methylbenzene, A new synthetic method of this compound is introduced below., Formula: C10H14O3

To a two-necked round-bottom flask containing a solution of (CH2O)n (0.030 g, 1 mmol) and HCl (37%, 0.5 mL) in AcOH (5 mL) was added, by means of a syringe pump (rate=10 mL/h), a solution of 3,4,5-trimethoxy-toluene (0.182 g, 1 mmol) in AcOH (5 mL) over a period of 30 min at 20 C. The solution was stirred for another 30 min. The mixture was then poured into EtOAc (40 mL) and washed with H2O (1×40 mL) and a saturated NaHCO3 aqueous solution (3×40 mL). The organic layer was dried (Na2SO4), filtered, and concentrated in vacuo to give a transparent oil (0.209 g) containing 2-chloromethyl-3,4,5-trimethoxytoluene in 77% yield, and 2,2′,3,3′,4,4′-hexamethoxy-6,6′-dimethylbiphenyl-methane (23%) as the main by-product. Purification of 2-chloromethyl-3,4,5 trimethoxytoluene by alumina or silica gel chromatography was fruitless since 2-chloromethyl-3,4,5-trimethoxytoluene, in the presence of traces of H2O, reacted to give the corresponding benzyl alcohol. Using the NMR spectra of a pure sample of 2,2′,3,3′,4,4′-hexamethoxy-6,6′-dimethylbiphenylmethane as reference (see Supporting Information in Appendix E), the characteristic signals of 2-chloromethyl-3,4,5-trimethoxytoluene were detected in the NMR spectra of the final reaction mixture. 1H NMR (200 MHz, CDCl3, ppm): delta2.37 [s, 3H, CH3], 3.84-3.96 [9H, 3×OCH3], 4.68 [s, 2H, CH2], 6.52 [s, 1H, ArH]. 13C NMR (200 MHz, CDCl3, ppm): delta18.7, 38.6, 55.7, 60.6, 61.4, 109.3, 121.9, 133.4, 140.0, 152.2, 153.4. MS m/z (%): 230 (31), 215 (1), 195 (100), 180 (40), 165 (5), 150 (12), 137 (12), 120 (6), 105 (7), 91 (5), 77 (6), 66 (5).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Bjorsvik, Hans-Rene; US2008/287702; (2008); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 6443-69-2, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 6443-69-2, name is 1,2,3-Trimethoxy-5-methylbenzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Compound 1 (3.6 g, 20 mmol) and NaBr (2.2 g, 20 mmol) were dissolved in HOAc (10 mL). The mixture was treated dropwise with 30% H2O2 (2.4 mL, 20 mmol) at room temperaturefor 1 h. Then, the mixture was quenched with water (8 mL) and extracted with diethyl ether (3 × 10 mL). The combined organic phases were washed with saturated NaHCO3 (3 × 5 mL) until pH 7, the combined the organic layers were dried over anhydrous Na2SO4, and evaporatedin vacuo to afford yellow oil 2 (5.2 g) in quantitative yield. 1H NMR (400 MHz, CDCl3): delta 6.61 (s, 1H, ArH), 3.89(s, 3H, OCH3), 3.86 (s, 3H, OCH3), 3.84 (s, 3H, OCH3),2.37 (s, 3H, CH3). 13C NMR (101 MHz, CDCl3): delta 152.2, 150.8, 141.1,133.4, 110.8, 109.5, 61.1 (OCH3), 60.9 (OCH3), 56.1(OCH3), 23.2(CH3). Spectroscopic data are according to the literature (Wanget al. 2016).

The synthetic route of 1,2,3-Trimethoxy-5-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Qiu, Yong-Fu; Lu, Bin; Yan, Yi-Yu; Luo, Wan-Yue; Wang, Jin; Hu, Xiao; Chemical Papers; vol. 73; 11; (2019); p. 2745 – 2748;,
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Reference of 6443-69-2, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 6443-69-2 name is 1,2,3-Trimethoxy-5-methylbenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Reference Example 3 To a solution of 18-acetoxy-n-octadecanoyl chloride (11 g) in 1,2-dichloroethane (50 ml) is added aluminum chloride (7 g) and the mixture is stirred at room temperature for 2 hours. This reaction mixture is cooled to 5 C. and a solution of 3,4,5-trimethoxytoluene (6.2 g) in 1,2-dichloroethane (20 ml) is added. The mixture is stirred at room temperature for 72 hours. Then, this reaction mixture is heated to 50 C.-60 C. and stirred for 30 minutes. After cooling, ice-water is added to the reaction mixture and the product is extracted with dichloromethane. The dichloromethane layer is washed with water and the solvent is distilled off to recover an oil (12.1 g). This oil is dissolved in methanol (150 ml) followed by addition of sodium hydroxide (5.2 g). The mixture is stirred at room temperature for 2 hours, at the end of which time it is neutralized with 5N–HCl and the solvent is distilled off. The resultant crude crystals are rinsed with water and recrystallized from dichloromethane-ether (1:1). The above procedure yields 6-(18-hydroxy-1-oxooctadecyl)-2,3-dimethoxy-5-methylphenol (6.4 g) as colorless needles, m.p. 101 C. Elemental analysis for C27 H46 O5. Calcd. C, 71.96; H, 10.29. Found C, 72.08; H, 10.51.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,2,3-Trimethoxy-5-methylbenzene, and friends who are interested can also refer to it.

Reference:
Patent; Takeda Chemical Industries, Ltd.; US4495104; (1985); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

These common heterocyclic compound, 6443-69-2, name is 1,2,3-Trimethoxy-5-methylbenzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Application In Synthesis of 1,2,3-Trimethoxy-5-methylbenzene

Eine Loesung von 1047 g (3,973 mol) 5-Brom-2-methoxy-6-methylben- ZOESaeURECHLORID in 1715 g Chlorbenzol wurden mit 0,72 g (0,0044 mol) (Beispiele 1 bis 4und 7) bzw. 0,36 g (0,0022 mol) (Beispiel 5) bzw. 0,18 g (0,0011 mol) (Beipiel 6) wasserfreiem Eisen- (III) chlorid versetzt und zu einer Loesung von 868,7 g (4,768 mol) 3,4, 5-Trimethoxytoluol in 467,8 g Chlorbenzol bei der in der Tabelle angegebenen Reaktionstemperatur waehrend 4 h dosiert. An- schliessend wurde das Reaktionsgemisch 2 h bei Reaktionstemperatur nachgeruehrt. Zur Entfernung der entstandenen HC1 wurde waehrend der Dosier-und Nachruehrzeit ein konstanter Stickstoffstrom durch das Reaktionsgemisch geleitet (der jeweilige Volumenstrom kann der Tabelle entnommen werden). Anschliessend wurde das Chlorbenzol bei 80 mbar und Temperaturen von 80-105C abdestilliert. Reinheit und Ausbeute der rohen Produktschmelze wurden vor Kristallisation mittels quantitativer HPLC analysiert (Ergebnisse siehe Tabelle). Zur Kristallisation des 5-Bromo-2′, 6-dimethyl-2,4′, 5′, 6′-tetrame- thoxybenzophenons (I’) wurden 4900 g Methanol bei 50C vorgelegt und die 105C heisse Schmelze eingetragen. Die Kristallisation er- folgte durch Abkuehlung mittels einer Temperaturrampe bis AUF-5C. Die Titelverbindung wurde durch Zentrifugation isoliert, auf der Zentrifuge mit Methanol gewaschen und getrocknet.

The synthetic route of 1,2,3-Trimethoxy-5-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BASF AKTIENGESELLSCHAFT; WO2004/54953; (2004); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Some common heterocyclic compound, 6443-69-2, name is 1,2,3-Trimethoxy-5-methylbenzene, molecular formula is C10H14O3, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: 6443-69-2

Compound 1 (1.82 g, 0.01 mol), NaBr (1.13 g, 0.011 mol) and sulfuric acid (2 mL) weredissolved in ethanol (8 mL). The mixture was treated dropwise with 30% H2O2 (5 mL,0.045 mol) at room temperature over a period of 1 h. Then the mixture was quenchedwith water (10 mL) and extracted with petroleum ether (15mL 3). The organic layerswere combined and evaporated in vacuo to afford 2, 2.60 g, 100%, yellowish oil.IR: (cm1) 3490, 2934, 1570, 1466, 1402, 1109, 824. 1H NMR (400MHz, CDCl3):d 6.61 (s, 1H, ArH), 3.89 (s, 3H, OCH3), 3.86 (s, 3H, OCH3), 3.84 (s, 3H, OCH3),2.37 (s, 3H, CH3). 13C NMR (101 MHz, CDCl3): d 152.2, 150.8, 141.1, 133.4, 110.8,109.5, 61.1 (OCH3), 60.9 (OCH3), 56.1 (OCH3), 23.2(CH3). The spectroscopic data arein accord with the literature.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 6443-69-2, its application will become more common.

Reference:
Article; Qiu, Yong-Fu; Yan, Yi-Yu; Lu, Bin; Tang, Lei; Zhai, Yu-Lin; Chen, Ke-Xin; Wang, Jin; Organic Preparations and Procedures International; vol. 51; 6; (2019); p. 602 – 605;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 6443-69-2, name is 1,2,3-Trimethoxy-5-methylbenzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 6443-69-2

3,4,5-Trimethoxytoluene (1.82 g, 10 mmol) was dissolvedin a mixture of acetic acid (10 mL) and catalytic H2SO4 (0.01 mL), then a solution of the oxidant (15 mmol) was added dropwise over 10 min. The mixture was stirred and heated at 50C for 1 h. After cooling, the reaction mixture was extracted with CH2Cl2 (3 × 10 mL). The combined organic phases were washed with H2O and NaHCO3, then dried over anhydrous Na2SO4 and evaporated under reduced pressure. The residue was purified by silica gel column chromatography (PE/EtOAc, 5:1) to give CoQ0. CoQ0, red-colored needles, m.p. 55C-58C (Lit.1357C-59C).1H NMR (400 MHz, CDCl3): delta = 6.44 (q, J = 1.7 Hz, 1H),4.02 (s, 3H, OCH3), 4.00 (s, 3H, OCH3), 2.04 (d, J = 1.6 Hz,3H, CH3).13C NMR (101 MHz, CDCl3): delta = 184.4 (C=O), 184.2(C=O), 145.0, 144.8, 144.0, 131.2, 61.2 (OCH3), 61.1(OCH3), 15.4 (CH3).MS (ESI): m/z = 205 [M + Na]+.The spectroscopic data are in accord with the literature.

The synthetic route of 6443-69-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Lu, Bin; Qiu, Yong-Fu; Qi, Shi; Wang, Jin; Journal of Chemical Research; vol. 43; 11-12; (2019); p. 553 – 556;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 6443-69-2, name is 1,2,3-Trimethoxy-5-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C10H14O3

REFERENCE EXAMPLE 5 To a solution (50 ml) of 18-acetoxy-n-octadecanoyl chloride (11 g) in 1,2-dichloroethane is added aluminum chloride (7 g), and the mixture is stirred at room temperature for 2 hours. The reaction mixture is cooled to 5 C., followed by addition of a solution (20 ml) of 3,4,5-trimethoxytoluene (6.2 g) in 1,2-dichloroethane. The whole mixture is stirred at room temperature for 72 hours. Further, the reaction mixture is heated to 50-60 C. and stirred for 30 minutes. After cooling, ice water is added and the product is extracted with dichloromethane. The dichloromethane layer is washed with water and the solvent is distilled off to give an oil (12.1 g). The oil is dissolved in methanol (150 ml) followed by addition of sodium hydroxide (5.2 g) and stirring at room temperature for 2 hours. The reaction mixture is neutralized with 5 N hydrochloric acid and the solvent is distilled off to give crude crystals. Washing the product with water and recrystallization from dichloromethane-ether (1:1) give colorless needles of 6-(18-hydroxy-1-oxooctadecyl)-2,3-dimethoxy-5-methylphenol (6.4 g). m.p. 101 C.

According to the analysis of related databases, 6443-69-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Takeda Chemical Industries, Ltd.; US4436753; (1984); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 6443-69-2, name is 1,2,3-Trimethoxy-5-methylbenzene, A new synthetic method of this compound is introduced below., Computed Properties of C10H14O3

To a two-necked round-bottom flask containing a solution of (CH2O)n (0.030 g, 1 mmol) and HCl (37%, 0.5 mL) in AcOH (5 mL) was added, by means of a syringe pump (rate=10 mL/h), a solution of 3,4,5-trimethoxy-toluene (0.182 g, 1 mmol) in AcOH (5 mL) over a period of 30 min at 20 C. The solution was stirred for another 30 min. The mixture was then poured into EtOAc (40 mL) and washed with H2O (1×40 mL) and a saturated NaHCO3 aqueous solution (3×40 mL). The organic layer was dried (Na2SO4), filtered, and concentrated in vacuo to give a transparent oil (0.209 g) containing 2-chloromethyl-3,4,5-trimethoxytoluene in 77% yield, and 2,2′,3,3′,4,4′-hexamethoxy-6,6′-dimethylbiphenyl-methane (23%) as the main by-product. Purification of 2-chloromethyl-3,4,5 trimethoxytoluene by alumina or silica gel chromatography was fruitless since 2-chloromethyl-3,4,5-trimethoxytoluene, in the presence of traces of H2O, reacted to give the corresponding benzyl alcohol. Using the NMR spectra of a pure sample of 2,2′,3,3′,4,4′-hexamethoxy-6,6′-dimethylbiphenylmethane as reference (see Supporting Information in Appendix E), the characteristic signals of 2-chloromethyl-3,4,5-trimethoxytoluene were detected in the NMR spectra of the final reaction mixture. 1H NMR (200 MHz, CDCl3, ppm): delta2.37 [s, 3H, CH3], 3.84-3.96 [9H, 3×OCH3], 4.68 [s, 2H, CH2], 6.52 [s, 1H, ArH]. 13C NMR (200 MHz, CDCl3, ppm): delta18.7, 38.6, 55.7, 60.6, 61.4, 109.3, 121.9, 133.4, 140.0, 152.2, 153.4. MS m/z (%): 230 (31), 215 (1), 195 (100), 180 (40), 165 (5), 150 (12), 137 (12), 120 (6), 105 (7), 91 (5), 77 (6), 66 (5).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Bjorsvik, Hans-Rene; US2008/287702; (2008); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Reference of 6443-69-2,Some common heterocyclic compound, 6443-69-2, name is 1,2,3-Trimethoxy-5-methylbenzene, molecular formula is C10H14O3, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: BF3¡¤Et2O was slowly added dropwise, to a stirred solution of polyhydroxy or polymethoxy phenols and alkyl alchol in dioxane at 0C. After the addition was completed, the stirring was continued for 3h at room temperature. The mixture was poured water and extracted with EtOAc. The organic layer was dried over Na2SO4 and filtered. The solvent was evaporated under reduced pressure. The crude was chromatographed on silica gel.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,2,3-Trimethoxy-5-methylbenzene, its application will become more common.

Reference:
Article; Kamauchi, Hitoshi; Oda, Takumi; Horiuchi, Kanayo; Takao, Koichi; Sugita, Yoshiaki; Bioorganic and Medicinal Chemistry; vol. 28; 1; (2020);,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 6443-69-2, name is 1,2,3-Trimethoxy-5-methylbenzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: ethers-buliding-blocks

General procedure: A pyrex test tube containing solid of 1,3,5-trimethoxybenzene (1a, 0.3 mmol), carbon tetrabromide (0.075 mmol), AQN-2-CO2H (0.03 mmol) and dry EtOH (5 mL) was irradiated for 20 h at roomtemperature with stirring by a 21W fluorescent lamp under air. The reactionmixture was concentrated in vacuo, quenched with aq Na2S2O3 and extractedwith EtOAc. The organic layer was dried over MgSO4 and concentrated invacuo. Purification of the residue by flash chromatography on silica gel(hexane/ethyl acetate = 6:1) provided 2-bromo-1,3,5-trimethoxybenzene (2a)(66.8 mg, 90%,) as a white solid.

The synthetic route of 6443-69-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Tanaka, Masanori; Kamito, Yuji; Lei, Cui; Tada, Norihiro; Itoh, Akichika; Tetrahedron Letters; vol. 56; 43; (2015); p. 5886 – 5888;,
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