Month: May 2021

Related Products of 37466-89-0,Some common heterocyclic compound, 37466-89-0, name is 3-Methoxybenzene-1,2-diamine, molecular formula is C7H10N2O, 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.

A mixture of 2-methoxy-6-nitroaniline (1 g, 5.95 mmol), 10% palladium carbon (300 mg) and methanol (25 ml) was stirred in a hydrogen atmosphere for 4 hours. The reaction vessel was purged with nitrogen and a catalyst was removed by filtration. To the reaction mixture, carbon disulfide (15 ml) was added and the mixture was stirred at room temperature overnight. Triethylamine (1 ml) was added to the reaction mixture, which was stirred at 50 C. for 3 hours. After the reaction mixture was concentrated, methanol (2 ml) and diethyl ether (20 ml) were added to the residue. The generated solid was collected by filtration to obtain the title compound (950 mg, yield: 88.6%) as a light orange solid.

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

Reference:
Patent; Eisai Co., Ltd.; US2007/10542; (2007); A1;,
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Related Products of 2062-98-8,Some common heterocyclic compound, 2062-98-8, name is Perfluoro(2-methyl-3-oxahexanoyl) fluoride, molecular formula is C6F12O2, 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.

In the implementation of the example 1 on the basis of the, to amplify production test: the full the fluorine is positive n-propyl vinyl ether (PPVE) 1 kg, hexafluoropropylene oxide dimer 1.5 kg, cesium fluoride 120g and diethylene glycol dimethyl ether 2.6L adding 10L in the reactor, the temperature is increased to 95 C, stirring for 2 hours, the reaction pressure will not change the observation, cooling, opening the reaction kettle, separating out the lower liquid product distillation is C11 the re-compounding process 1.95 kg, yield is 87%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Perfluoro(2-methyl-3-oxahexanoyl) fluoride, its application will become more common.

Reference:
Patent; Tianjin Changlu Chemical New Material Co., Ltd; Zhang, Zhijun; Zhao, Xinghua; Xu, Yashuo; Wang, Bo; Xiao, Shan; (5 pag.)CN105503552; (2016); A;,
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Electric Literature of 53087-13-1,Some common heterocyclic compound, 53087-13-1, name is 1-(Benzyloxy)-3-bromobenzene, molecular formula is C13H11BrO, 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.

Iodine, warmed up with magnesium, was added to a suspension of magnesium tunings (i .29 g,52.8 mmol) in dry THF (50 mL). The mixture was ref luxed and about 5% of a solution of 3-bromophenol (i3.9 g, 52.8 mmol) was added. When the reaction had started, the solution of the bromide was added drop-wise and the mixture was then ref luxed for one more hour. Themixture was cooled down to about 5 00 and a solution of the cyclopentanone (4.44 g, 52.8 mmol) in THF (50 mL) was added drop-wise. The mixture was stirred at rt for 72 h, then the reactio was quenched with cooled saturated ammonium chloride solution and extracted with diethyl ether (x3). The organic phase was washed with brine, dried (Na2SO4), filtered and concentrated. The product was purified by silica gel chromatography (isohexane / EtOAc),which gave the title compound (8.5 g, 54%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-(Benzyloxy)-3-bromobenzene, its application will become more common.

Reference:
Patent; MEDIVIR AB; KALAYANOV, Genadiy; TORSSELL, Staffan; WAeHLING, Horst; WO2015/34420; (2015); A1;,
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Synthetic Route of 22483-09-6, The chemical industry reduces the impact on the environment during synthesis 22483-09-6, name is 2,2-Dimethoxyethanamine, I believe this compound will play a more active role in future production and life.

(3,4-Methylenedioxybenzylidene)-(2,2-dimethoxyethyl)amine (11b). Aminoacetaldehyde dimethylacetal (7.10 g, 0.0666 mol) was dissolved in chloroform (50 mL) and MgSO4 (12 g) was added. Then piperonal (10b, 10.10 g, 0.0666 mol) was added and the mixture was stirred at room temperature. After 24 h there still was unreacted piperonal in the reaction mixture and more amine (6.00 g) was added. The reaction mixture was stirred again at room temperature for 24 h and since there still was some piperonal present more amine (6.00 g) was added again. After stirring the reaction mixture for another 24 h at room temperature the imine was isolated. The reaction mixture was diluted with water (300 mL) and the organic layer was washed with water 200 mL*2, brine (200 mL) dried Na2SO4 and concentrated to provide the pure imine as a yellow oil (15.80 g, 100%). 1H NMR (300 MHz, CDCl3) delta 8.13 (s, 1H), 7.33 (s, 1H), 7.07 (d, J=8.10 Hz, 1H), 6.78 (d, J=8.10 Hz, 1H), 5.96 (s, 2H), 4.62 (t, J=5.4 Hz, 1H), 3.70 (d, J=4.2, 2H), 3.83 (s, 6H).

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, 2,2-Dimethoxyethanamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Cushman, Mark S.; Ioanoviciu, Alexandra S.; Pommier, Yves G.; US2008/242692; (2008); A1;,
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Related Products of 2132-62-9,Some common heterocyclic compound, 2132-62-9, name is 1,2-Bis(4-methoxyphenyl)ethyne, molecular formula is C16H14O2, 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: In a oven-dried RBF, a solution of Imidazo[1,2,-a]pyridines derivatives 1 (0.5 mmol) and alkyne2 in toluene (2 mL) [Cp*RhCl2]2 (5 mol%), Cu(OAc)2·H2O (2 equiv), Cs2CO3 (30 mol%) wereadded under inert atmosphere. The resulting reaction mixture was heated at 125 C for 7 h.Progression of the reaction was monitored by TLC, while noticing complete consumption ofImidazo[1,2,-a]pyridines derivatives, reaction was brought to room temperature. The additionalamount of acrylate also added if required for complete conversion. The reaction mixture wasdiluted with ethyl acetate (10 mL) and water (15 mL) and then filtered through a plug of celite.The layers were separated, and the organic layer was washed with aqueous saturated brinesolution, dried over Na2SO4. Organic layer was concentrated under reduced pressure.The crudematerial so obtained was purified by column chromatography on silica gel (hexane: ethylacetate :: 70:30). The structure and purity of known starting materials were confirmed by comparison oftheir physical and spectral data (1H NMR, 13C NMR and HRMS ).

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-Bis(4-methoxyphenyl)ethyne, its application will become more common.

Reference:
Article; Kotla, Siva K. Reddy; Choudhary, Deepak; Tiwari, Rakesh K.; Verma, Akhilesh K.; Tetrahedron Letters; vol. 56; 32; (2015); p. 4706 – 4710;,
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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 6298-96-0 as follows. Computed Properties of C9H13NO

(a). ( 1 S)-JV- r 1 -(4-Methoxy-phenyl>ethyll -3 -oxo-butyramide; To a solution of (S)-l-(4-methoxy-phenyl)-ethylamine (25 g) in dichloromethane (60 mL) was added TEA (20 g) and DMPA (200 mg). Then a solution of 4-methylene- oxetan-2-one (16.7 g) in dichloromethane (60 ml) was added over a period of 30 minutes and then stirred at 20 0C for 18 h. The mixture was washed with IM HCl, aq. NaHCO3 and aq. NaCl. The organic layer was dried (MgSO4), filtered and concentrated in vacuo. EPO Yield: 39.8 g. MS-ESI: [M+H]+ = 236

According to the analysis of related databases, 6298-96-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; N.V. ORGANON; WO2006/117368; (2006); A1;,
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These common heterocyclic compound, 1663-61-2, name is (Triethoxymethyl)benzene, 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. name: (Triethoxymethyl)benzene

General procedure: Triethyl orthoformate, orthoacetate, orthopropionate or orthobenzoate(10 mmol) was added dropwise to the mixture of 1,2,4,5-tetrazine-3,6-dicarbohydrazide (6) (0.5 g, 2.5 mmol) and glacial aceticacid (7 mL). The reaction was carried out using conventional heating ormicrowave irradiation (150 W) in five cycles of 90 s with 2 min intervalsat the temperature 50-100 C.

The synthetic route of (Triethoxymethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; K?dzia, Anna; Kudelko, Agnieszka; ?wi?tkowski, Marcin; Kruszy?ski, Rafa?; Dyes and Pigments; vol. 172; (2020);,
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Application of 7664-66-6, 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. 7664-66-6, name is 4-Isopropoxyaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 54: Preparation of 2-[l-(4-fluorophenyl)-3-[2-(4-methoxyphenyl)ethyl]-5- oxo-2-sulfanylideneimidazolidin-4-yl]-N-[4-(propan-2-yloxy)phenyl]acetamide. – EDCI (143 mg; 0.74 mmol; 1.5 eq), followed by HOBt (113 mg; 0.74 mmol; 1.5 eq), DIPEA (256 muU 1-49 mmol; 3 eq) and 4-(propan-2-yloxy)aniline (150 mg; 0.99 mmol; 2 eq) were added to a solution of 2-[l-(4-fluorophenyl)-3-[2-(4- methoxyphenyl)ethyl] -5-oxo-2-sulfanylideneimidazolidin-4-yl] acetic acid (1-21 ) (200 mg; 0.50 mmol; 1 eq) in anhydrous dioxane (8 mL). The reaction mixture was stirred at room temperature for 18 hours. Saturated ammonium chloride (20 mL) was added and the aqueous layer was extracted with ethyl acetate (3 x 25 mL). The combined organic layers were washed with saturated sodium chloride (3 x 20 mL), dried over sodium sulfate, filtered and concentrated to dryness. The crude was purified on silica gel using dichloromethane/ethyl acetate (95/5) as an eluent. After trituration in diethyl ether/ethanol, the title compound 2-[l-(4-fluorophenyl)-3-[2-(4- methoxyphenyl)ethyl]-5-oxo-2-sulfanylideneimidazolidin-4-yl]-N-[4-(propan-2- yloxy)phenyl]acetamide was obtained with 43% yield (114 mg) as a white solid. 1H- NMR (Acetone-d6): delta (ppm), 1.26 (d, 6H), 2.94 (m, 1H), 3.15 (m, 2H), 3.36 (m, 1H), 3.74 (s, 3H), 3.78 (m, 1H), 4.31 (m, 1H), 4.59 (m, 2H), 6.86 (d, 4H) , 7.25 (m, 4H), 7.48 (m, 4H), 9.32 (s, 1H); MS (ESI+): m/z = 535.9 [M+H]+ .

The synthetic route of 4-Isopropoxyaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; VIVALIS; GUEDAT, Philippe; BERECIBAR, Amaya; CIAPETTI, Paola; VENKATA PITHANI, Subhash; TROUCHE, Nathalie; WO2013/171281; (2013); A1;,
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767-91-9, name is 2′-Methoxyphenyl acetylene, belongs to ethers-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C9H8O

General procedure: Ferric sulfate hydrate (I, 8 mol%), glacial acetic acid (5 mL) and the alkyne (1 – 2 mmol) were introducedinto a 50 mL Schlenk tube, equipped with an air condenser, and the mixture kept under stirring at 95 C or120 C, until consumption of the substrate or no further conversion, as evidenced by TLC or GC. Uponcooling, the supernatant solution was poored into water and the residue washed twice with diethyl ether.After extraction with diethyl ether ( 2), the combined organic layers were washed with a saturated aqueoussolution of sodium bicarbonate and then water until neutrality. Alternatively, the crude from the reactions ofsubstrates featuring hydroxyl or carbonyl groups, as for 12, 15, 20 and 22, was obtained by removing aceticacid under vacuum, in order to reduce loss of material during biphasic extraction. The products were purified

The synthetic route of 767-91-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Bassetti, Mauro; Ciceri, Samuele; Lancia, Federico; Pasquini, Chiara; Tetrahedron Letters; vol. 55; 9; (2014); p. 1608 – 1612;,
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Some common heterocyclic compound, 29578-83-4, name is 1-Bromo-3-methoxy-5-methylbenzene, molecular formula is C8H9BrO, 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: 1-Bromo-3-methoxy-5-methylbenzene

A mixture of 5-bromo-3-methoxytoluene (20 g, 0.1 m), N-bromosuccinimide (17.8 g, 0.1 m) and dibenzoyl peroxide in carbon tetrachloride (200 ml) is heated to reflux and irradiated with a sunlamp. The mixture is cooled, filtered and concentrated in vacuo to give 5-bromo-3-methoxybenzyl bromide.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 29578-83-4, its application will become more common.

Reference:
Patent; SmithKline Beckman Corporation; US4659706; (1987); A;,
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