Tag: M.W=300-400

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. 162705-07-9, name is (Z)-2-Methoxy-5-(3,4,5-trimethoxystyryl)aniline, A new synthetic method of this compound is introduced below., COA of Formula: C18H21NO4

General procedure: The corresponding N-(1-oxyl-2,2,6,6-tetramethyl-4-piperidinyl-oxycarbonyl) amino acids 20a-h (0.47 mmol) were dissolved in 50 mL of anhydrous CH2Cl2 and cooled to 0 C. 1-Hydroxybenzotriazole (HOBt) (0.7 mmol) and EDCI (0.56 mmol) were added, and the mixture was stirred for 30 min at 0 C. Subsequently, 0.39 mmol of compound 3 and finally 2.4 mL of N-ethyl diisopropylamine were added. The mixture was stirred for 16 h at ambient temperature. The solvent was removed under reduced pressure and the residue was purified by flask-column chromatography (gradient elution with mixtures of chloroform/methanol) on silica gel as monitored by TLC. Synthesized target compounds 21a-h were characterized by mp, IR, ESR and HRMS analyses.

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:
Article; Liu, Ying-Qian; Li, Xiao-Jing; Zhao, Chun-Yan; Nan, Xiang; Tian, Jing; Morris-Natschke, Susan L.; Zhang, Zhi-Jun; Yang, Xiao-Ming; Yang, Liu; Li, Lin-Hai; Zhou, Xing-Wen; Lee, Kuo-Hsiung; Bioorganic and Medicinal Chemistry; vol. 21; 5; (2013); p. 1248 – 1256;,
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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. 2062-98-8, name is Perfluoro(2-methyl-3-oxahexanoyl) fluoride, A new synthetic method of this compound is introduced below., COA of Formula: C6F12O2

F[CF(CF3)CF2O]4CF(CF3)C(O)F, a precursor of hydrofluoroether F[CF(CF3)CF2O]5CH3, was formed by pentapolymerization of hexafluoropropylene oxide. To the reaction vessel, potassium fluoride (10.0 g), hexafluoropropylene oxide dimer (150.0 g) and diethylene glycol dimethyl ether (2.5 L) were added at 15 C under stirring.To the round bottom flask was introduced hexafluoropropylene oxide (830 g, 5.0 mol) over 1 hour.The lower layer of the acyl fluoride phase product is mainly composed of a hexafluoropropylene oxide tetramer, a hexafluoropropylene oxide pentamer and a hexafluoropropylene oxide hexamer, and the yield of the hexafluoropropylene oxide pentamer is 65%. The crude product was further purified by distillation to obtain a product of a hexafluoropropylene oxide pentamer having a purity of 99% as determined by gas chromatography, and used.In the next alkylation reaction. The structure of the product was characterized by infrared spectroscopy and 19F NMR.

The synthetic route of 2062-98-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Tianjin Changlu Chemical New Materials Co., Ltd.; Yan Rui; He Guangrui; (15 pag.)CN109608312; (2019); A;,
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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. 2062-98-8, name is Perfluoro(2-methyl-3-oxahexanoyl) fluoride, A new synthetic method of this compound is introduced below., Recommanded Product: 2062-98-8

To a 3 -neck flask equipped with a temperature probe, magnetic stir bar, water- cooled condenser, and addition funnel was charged sodium borohydride (16.0 g, 423 mmol), and tetraethylene glycol dimethyl ether (125 mL). 2,3,3,3-Tetrafluoro-2- (1,1,2,2,3, 3, 3-heptafluoropropoxy)propanoyl fluoride (100 g, 301 mmol) was added dropwise to the resultant mixture. After complete addition, the reaction mixture was heated to reflux and stirred overnight. The mixture was then allowed to cool to room temperature followed by the dropwise addition of methanol (100 mL) and H2O (150 mL). The mixture was then transferred to a separatory funnel and the fluorous phase was collected and then distilled (46.1 C, 40 ton) to afford 2,3,3,3-tetrafluoro-2-(l, 1,2,2,3,3- heptafluoropropoxy)propan-l-ol (67.5 g, 71%) as a colorless liquid. The isolated compound was used in the next step. (0204) To a 3-neck flask equipped with a temperature probe, distillation head, overhead stirrer, and under N2 was charged TiCU (7.9 mL, 72 mmol). 2,3,3,3-Tetrafluoro-2- (l,l,2,2,3,3,3-heptafluoropropoxy)propan-l-ol (15.1 g, 47.8 mmol) was added dropwise with stirring and the resultant mixture was heated to 40 C followed by a 30 min stir. The mixture was then allowed to cool to room temperature followed by the dropwise addition of tetraethylene glycol dimethyl ether (45 mL). Exotherms reaching approximately 50 C were observed. The resultant mixture was allowed to warm to room temperature followed by the addition of zinc dust (9.1 g, 140 mmol) in one portion. The resultant reaction mixture was raised to 85 C. After a 3 h stir, the temperature was slowly raised to 225 C and distillate was collected with the distillation head temperature reaching 69 C affording the title compound (4.1 g, 31%) as a colorless liquid.

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; 3M INNOVATIVE PROPERTIES COMPANY; SMITH, Sean M.; LAMANNA, William M.; COSTELLO, Michael G.; BULINSKI, Michael J.; (35 pag.)WO2017/195070; (2017); A1;,
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Synthetic Route of 2062-98-8, 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. 2062-98-8, name is Perfluoro(2-methyl-3-oxahexanoyl) fluoride belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 2; Example 2-1; [0175] Example for Preparation of CH2CHCH(OCH3) CH2OCOCF (CF3)OCF2CF2CF3; [0176] CH2CHCH(OCH3)CH2OH (270 g) was charged together with NaF (334 g) into a 2 L pressure resistant reactor equipped with a reflux condenser in which a coolant at 20 C. circulated, and stirred at -10 C. While discharging by-product HF formed by the reaction out of the system from the reflux condenser on the upper portion by bubbling nitrogen gas to the reactor, FCOCF(CF3)OCF2CF2CF3 (1055 g) was dropwise added over a period of 1.5 hours. At this time, the temperature was adjusted so that the internal temperature of the reactor would be at most 0 C. After completion of the dropwise addition, stirring was carried out at 30 C. for 18 hours and then the reaction was terminated. [0177] NaF contained in the crude liquid after completion of the reaction was collected by filtration to obtain a crude product (981 g) (yield 86.4%). As a result of the analysis by NMR, the above-identified mixture was obtained as a liquid mixture with FCOCF(CF3)OCF2CF2CF3. The results of analysis of the above-identified compound are as follows. [0178] 1H-NMR(300.4 MHz, solvent:CDl3, standard:TMS) delta (ppm):3.29(s, 3H), 3.85-3.90(m, 1H), 4.24-4.45(m, 2H), 5.34(s, 1H), 5.39(d,J=8.4 Hz, 1H), 5.59-5.71(m, 1H). [0179] 19F-NMR(282.7 MHz, solvent:CDCl3, standard:CFCl3) delta (ppm): -81. 8(3F), -82.6(3F), -79.9-87.5(2F), -130.2(2F), -132.3(1F).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Perfluoro(2-methyl-3-oxahexanoyl) fluoride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASAHI GLASS COMPANY LIMITED; US2003/216595; (2003); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Application of 162705-07-9,Some common heterocyclic compound, 162705-07-9, name is (Z)-2-Methoxy-5-(3,4,5-trimethoxystyryl)aniline, molecular formula is C18H21NO4, 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: DCC (0.47 mmol, 1.2 eq.); the N-Fmoc-protected amino acid (0.472 mmol, 1.2 eq) and HOBt·H2O (0.47 mmol, 1.2 eq) were added to a solution of the 30-aminocombretastatin (0.39 mmol, 1 eq) in anhydrous DMF (1.3 mL). The reaction mixture was stirred under N2 atmosphere for 16 h. Then, it was ltered, and the ltrate was poured into a saturated aqueous NH4Cl solution and then extracted with AcOEt (3×15 mL). The combined organic extracts were washed 2 times with water and brine and dried over anhydrous MgSO4. After ltration and evaporation of the solvent under reduced pressure, the resulting residue was chromatographed on silica gel with Hexanes-AcOEt (6:4) to aord the corresponding N-Fmoc-protected derivatives 7 and 9.

The synthetic route of 162705-07-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Agut, Rauel; Alberto Marco, J.; Carda, Miguel; Falomir, Eva; Gil-Edo, Raquel; Martin-Beltran, Celia; Murga, Juan; Pla, Alberto; Molecules; vol. 25; 3; (2020);,
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. 162705-07-9, name is (Z)-2-Methoxy-5-(3,4,5-trimethoxystyryl)aniline, A new synthetic method of this compound is introduced below., Recommanded Product: (Z)-2-Methoxy-5-(3,4,5-trimethoxystyryl)aniline

Example 8 (Z)-1-(3-hydroxy-4-methoxyphenyl)-3-((2-methoxy-5-((Z)-3,4,5-trimethoxystyryl)phenyl)amino) prop-2-en-1-one (10q) To a stirred solution of (Z)-2-methoxy-5-(3,4,5-trimethoxystyryl)aniline (5d) (100 mg, 0.317 mmol) in ethanol (5 ml) 1-(3-hydroxy-4-methoxyphenyl)prop-2-yn-1-one (6q) (55.85 mg, 0.317 mmol) was added. The reaction mixture was stirred at a temperature of 24 C. for 4 h and the reaction was monitored by TLC using hexane/ethyl acetate (6:4) as a solvent system. Then appropriate water was added to reaction mixture. A yellow colour solid appears which was filtered and washed with ethanol. (yield: 110 mg, 70%); mp: 88-91 C.; 1H NMR (CDCl3, 300 MHz) deltadelta (ppm): 3.71 (s, 6H), 3.85 (s, 3H), 3.94 (s, 6H), 5.68 (s, 1H), 5.91 (d, J=8.3 Hz, 1H), 6.49 (d, J=13.6 Hz, 4H), 6.79 (d, J=8.3 Hz, 1H), 6.96-6.87 (m, 2H), 7.12 (s, 1H), 7.24-7.18 (m, 1H), 7.50 (d, J=6.7 Hz, 2H), 12.06 (d, J=12.1 Hz, NH); FABMAS:(M+H)=478.

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; Council of Scientific and Industrial Research; Ahmed, Kamal; Gajjela, Bharath Kumar; Anver, Basha Shaik; Vangala, Santhosh Reddy; Mahesh, Rasala; US2015/322009; (2015); A1;,
Ether – Wikipedia,
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In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 2062-98-8 as follows. name: Perfluoro(2-methyl-3-oxahexanoyl) fluoride

Under a nitrogen atmosphere, ethyl 3-dimethylam- inoethyl acrylate (1.43 g) was dissolved in toluene (10 ml), and pyridine (0.8 g) was added at room temperature. Perfluoro(1 -(1 -propoxy) propionic acid) fluoride (perfluoro(2- methyl-3-oxa-hexanoyl) fluoride) (3.2 g) was dropwise added thereto, followed by stirring for 10 hours at the same temperature. Water (20 ml) was added to the reaction mixture, and the organic phase was separated. Further, the aqueous phase was extracted with toluene (10 ml), and the extract was combined with the previous organic phase. This organic phase was dried over anhydrous magnesium sulfate, and the solvent was distilled oil to obtain 4.5 g of a compound represented by the following formula.

According to the analysis of related databases, 2062-98-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ASAHI GLASS COMPANY, LIMITED; MORIZAWA, Yoshitomi; TAKAHIRA, Yusuke; (32 pag.)US2016/295864; (2016); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

These common heterocyclic compound, 162705-07-9, name is (Z)-2-Methoxy-5-(3,4,5-trimethoxystyryl)aniline, 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. Recommanded Product: 162705-07-9

General procedure: DCC (0.47 mmol, 1.2 eq.); the N-Fmoc-protected amino acid (0.472 mmol, 1.2 eq) and HOBt·H2O (0.47 mmol, 1.2 eq) were added to a solution of the 30-aminocombretastatin (0.39 mmol, 1 eq) in anhydrous DMF (1.3 mL). The reaction mixture was stirred under N2 atmosphere for 16 h. Then, it was ltered, and the ltrate was poured into a saturated aqueous NH4Cl solution and then extracted with AcOEt (3×15 mL). The combined organic extracts were washed 2 times with water and brine and dried over anhydrous MgSO4. After ltration and evaporation of the solvent under reduced pressure, the resulting residue was chromatographed on silica gel with Hexanes-AcOEt (6:4) to aord the corresponding N-Fmoc-protected derivatives 7 and 9.

The synthetic route of (Z)-2-Methoxy-5-(3,4,5-trimethoxystyryl)aniline has been constantly updated, and we look forward to future research findings.

Reference:
Article; Agut, Rauel; Alberto Marco, J.; Carda, Miguel; Falomir, Eva; Gil-Edo, Raquel; Martin-Beltran, Celia; Murga, Juan; Pla, Alberto; Molecules; vol. 25; 3; (2020);,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Some common heterocyclic compound, 105404-89-5, name is 2,7-Dibromo-3,6-dimethoxynaphthalene, molecular formula is C12H10Br2O2, 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 2,7-Dibromo-3,6-dimethoxynaphthalene

0.125 mol [intermediate 1-1] at room temperature,43.4 g and (4-chloro-2-fluorophenyl) boronic acid 0.301 mol, 52.5 g and Ce2CO3 0.815 mol, 266 g and TTP (tetrakis(triphenylphosphine)palladium(0)) 8 mol% 11.6 g was added with 500 mL of 1,4-dioxane and refluxed. After 4 hours, the reaction was cooled to room temperature, 500 ml of H2O was added, and extracted with EA.After filtration, the obtained solid was recrystallized from EA (ethyl acetate) and Hx (normal hexane) to obtain 0.09 mol of [Intermediate 1-2] and 41.0 g (yield 73%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 105404-89-5, its application will become more common.

Reference:
Patent; LG Chem, Ltd.; Gu Gi-dong; Kim Myeong-gon; Keum Su-jeong; Yoon Jeong-min; (52 pag.)KR2019/111688; (2019); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 2062-98-8 as follows. category: ethers-buliding-blocks

To a solution of hydroxyacetone (7.4 g) and pyridine (8.1 ml) in ethyl acetate (100 ml), undecafluoro-(2-methyl-3-oxahexanoic acid)fluoride (10 g) was added dropwise at room temperature (25 C.). After stirring at room temperature for 2 hours, the reaction mixture was poured into diluted hydrochloric acid. After separation, the organic layer was washed with water and a saturated sodium chloride solution and dried with magnesium sulfate. The concentrated residue was purified by column chromatography (developing solvent: ethyl acetate/hexane), to obtain Compound B (10.2 g, 88%).1H NMR (CDCl3) delta 2.22 (s, 3H), 4.85 (d, J=16.2 Hz, 1H), 4.96 (d, J=16.2 Hz, 1H)19FNMR (CDCl3) delta -80.3 (1F), -81.8 (3F), -82.5 (3F), -86.7 (1F), -130.2 (2F), -132.8 (1F)

According to the analysis of related databases, 2062-98-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; FUJIFILM Corporation; US2009/18350; (2009); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem