Month: February 2021

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 54149-17-6 as follows. Application In Synthesis of 1-Bromo-2-(2-methoxyethoxy)ethane

Syntheses of Monofunctional Azides:1-Azido-2-(2-methoxyethoxy)ethane, 19. A solution of 1-bromo-2-(2-methoxyethoxy) ethane (12.4 g, 67.8 mmol) and sodium azide (13.2 g, 203 mmol) in water (150 ml) was stirred under reflux for 16 hours. The aqueous phase was extracted with dichloromethane (2¡Á200 ml), dried with MgSO4 and evaporated to dryness, to give 19 as a colorless oil in 87.3% yield. 1H NMR (500 MHz, CDCl3): delta=3.29 (s, CH3O, 3H), 3.30 (t, J=5.2 Hz, CH2N3, 2H), 3.44-3.48 (m, CH3OCH2, 2H), 3.53-3.60 (m, CH2OCH2, 4H). 13C NMR (125 MHz, CDCl3): delta=50.89 (s, CH2N3, 1C), 59.27 (s, CH3O, 1C), 70.29 (s, CH3OCH2CH2, 1C), 70.84 (s, CH3OCH2CH2, 1C), 72.21 (s, CH2CH2N3, 1C).

According to the analysis of related databases, 54149-17-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; The Scripps Research Institute; US2009/69561; (2009); A1;,
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Related Products of 30568-44-6, 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. 30568-44-6, name is 2-(4-Methoxyphenyl)propan-2-amine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: (3S,4S)-4-{[4-(1H-Benzimidazol-2-yl)piperazin-1-yl]carbonyl}-3-(thiophen-3-yl)cyclohexanone (30 mg, 0.07 mmol) was dissolved in a mixture of MeOH (367 muL) and DCE (367 muL), and 2-(4-methoxyphenyl)propan-2-amine (59.2 mg, 0.29 mmol) was added followed by MP-cyanoborohydride (159 mg, 0.367 mmol) and acetic acid (13.0 muL, 0.22 mmol) at rt. The reaction mixture was shaken overnight at 55 C, cooled to rt, filtered and concentrated under vacuum. LC-MS indicated a 3:2 ratio of diastereomeric reductive amination products.

The synthetic route of 2-(4-Methoxyphenyl)propan-2-amine has been constantly updated, and we look forward to future research findings.

Reference:
Article; Anthony Romero; Hastings, Nicholas B.; Moningka, Remond; Guo, Zhiqiang; Wang, Ming; Di Salvo, Jerry; Lei, Ying; Trusca, Dorina; Deng, Qiaolin; Tong, Vincent; Terebetski, Jenna L.; Ball, Richard G.; Ujjainwalla, Feroze; Bioorganic and Medicinal Chemistry Letters; vol. 22; 2; (2012); p. 1014 – 1018;,
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Application of 437-83-2, 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 437-83-2 as follows.

Compound 123: 4-(9-Cyclopentyl-7,7-difluoro-5-methyl-6-oxo-6,7,8,9- tetrahydro-5H-pyrimido[4,5-b][l,4]diazepin-2-ylamino)-2-fluoro-3-methoxybenzoic acid; [0590] 4-Bromo-3-fluoro-2-methoxyaniline: To 3-fluoro-2-methoxyaniline (2.8 g, 20 mmol) in 10 mL of acetic acid was added bromine (0.82 mL, 16 mmol) in acetic acid (10 rnL) dropwise. The reaction mixture was stirred at rt. for 30 min. Solid was filtered and washed with acetic acid to give the HBr salt. It was then dissolved in water, basified by addition of KOH, extracted with ethyl acetate. The organic layer was dried and concentrated to give a white solid (2.8 g, 80 %). 1U NMR (400 MHz, CHLOROFORM-J) delta ppm 3.93 (s, 3 H) 6.42 (dd, J=S.6, 1.8 Hz, 1 H) 7.01 (dd, J=8.6, 7.1 Hz, 1 H). [M+H] calc’d for C7H7BrFNO, 222; found 222.

According to the analysis of related databases, 437-83-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; WO2009/42711; (2009); A1;,
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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. 5961-59-1, name is 4-Methoxy-N-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., name: 4-Methoxy-N-methylaniline

4-Acetyl-N-(4-methoxy-phenyI)-N-methyl-benzamide 152. To a stirred solution of 4-acetylbenzoic acid (0.164 g, 1 mmol) and N-methyl-j?-anisidine (0.165 g, 1.2 mmol) in dry DCM (5 mL) and NEt3 (0.17 mL) was added DMAP (catalytic) and the solution was cooled on ice. To this was then added EDCI (0.383 g, 2 mmol) and the reaction was allowed to warm to rt with stirring over 22 h. To this was added sat. aq. bicarb, and DCM and the organic layer was separated and concentrated under reduced pressure. Purification by flash chromatography using an elution gradient of hexane to 30percent EtOAc in hexane gave the title compound, 0.186 g5 66 percent: 1H NMR delta (400 MHz, CDCl3) 2.47 (3H5 s), 3.40 (3H, s), 3.66 (3H5 s), 6.67 (2H5 d, J= 8.6 Hz), 6.89 (2H, d, J= 8.2 Hz)5 7.31 (2H, d5 J= 7.8 Hz)5 7.69 (2H5 d5 J= 7.8 Hz); 13C NMR delta (100 MHz, CDCl3) 26.5, 38.2, 55.2, 114.3, 127.5, 127.9, 128.5, 136.9, 137.0, 140.4, 158.0, 169.5, 197.4; LC/MS (APCI) m/z 304.47 (M-H)-; HPLC tT = 3.61 min (>99percent) 90percent MeCN m H2O.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 5961-59-1.

Reference:
Patent; STERIX LIMITED; WO2007/96647; (2007); A2;,
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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. 101-84-8, name is Diphenyl oxide, A new synthetic method of this compound is introduced below., Recommanded Product: 101-84-8

(1) diphenyl ether (44.2 g, 0.26 mol) was added into a 250 ml four-necked flask and 123.5 g (1.25 mol) of dichloroethane was added and stirred for 1 hour.Cool to -5 ~ 0 ,Bromine (21 g, 0.13 mol) was rapidly added dropwise and stirred for 1 hour. The mixture was cooled to -5~0 C and 30% hydrogen peroxide (15 g, 0.13 mol)With 0.5 to 1 hour dropwise addition and termination,The temperature is controlled between 0 and 5 DEG C, naturally heated to 25 DEG C after dropping, incubated for 32 hours between 27 DEG C and quenched with 49g of 15% sodium bisulfite, after the phase separation,Then washed with water to neutral, to distill dichloroethane distillation, distillation under reduced pressure before recovery of diphenyl ether, and finally collected 4-bromo-diphenyl ether 51.7g, yield 80.0%, content of 98.2%.

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; Binhai Extensive Chemical Co., Ltd.; Wu Fucai; (8 pag.)CN106957220; (2017); A;,
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These common heterocyclic compound, 16452-01-0, name is 3-Methoxy-4-methylaniline, 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: 3-Methoxy-4-methylaniline

To 6.05 g of dichlorophenylborane dissolved in 40 ml of dichloromethane, at -20 C., are successively added 5.226 g of 3-methoxy-4-methylaniline dissolved in 50 ml of dichloromethane, and 13.4 ml of triethylamine dissolved in 25 ml of dichloromethane. After 30 minutes at -20 C., 5.412 g of 2,6-difluorobenzaldehyde dissolved in 60 ml of dichloromethane are introduced. After 24 hours at room temperature, the mixture is hydrolyzed with water. The organic phase is dried over anhydrous sodium sulfate and concentrated. To the oil obtained, dissolved in 80 ml of diethyl ether, are added 80 ml of 2 M sodium hydroxide solution and the mixture is left stirring for 18 hours. The phases are separated by settling and the organic phase is dried over anhydrous sodium sulfate and concentrated. The residue is solidified with n-pentane to give 5.069 g of the expected product. 1H NMR delta in ppm (DMSO d6): 1.98 (s, 3H); 3.69 (s, 3H); 4.74 (s, 2H); 5.79 (d, 1H); 5.98 (d, 1H); 6.30 (s, 1H); 6.75 (s, 1H); 7.06 (m, 2H); 7.41 (m, 1H).

The synthetic route of 3-Methoxy-4-methylaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SANOFI-AVENTIS; US2007/185136; (2007); A1;,
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Electric Literature of 126829-31-0, The chemical industry reduces the impact on the environment during synthesis 126829-31-0, name is 2-Ethynyl-1,3-dimethoxybenzene, I believe this compound will play a more active role in future production and life.

Example 29; [0139] l,3-Bis(2,6-diisopropylphenyl)-4-(2,6-dimethoxyphenyl)-lH-l,2,3-triazolium hexafluorophosphate (lOal). To a stirred suspension of triazene 8a (3.66 g, 10 mmol), 2,6- dimethoxyphenylacetylene 91 (3.24 g, 20 mmol), and anhydrous potassiumhexafluorophosphate (1.84 g, 10 mmol) in dry dichloromethane (50 mL) in the dark at -78C is added tert-butyl hypochlorite (1.66 mL, 15 mmol), upon which the mixture instantly darkens. The mixture is stirred overnight as it is slowly allowed to warm to roomtemperature. The contents are then filtered, and the solid residue is washed withdichloromethane. The filtrate is collected, and volatiles are evaporated under reduced pressure. Diethyl ether is then added, and the mixture is vigorously triturated for ca. Ihour, with occasional scratching of the glass surfaces to ensure efficient mixing. Filtration and washing with copious quantities of diethyl ether afford, after drying under vacuum, triazolium salt lOai as an off-white solid (5.25 g, 78%). Analytical samples were obtained after recrystallization by vapor diffusion of diethyl ether in an acetonitrile solution of lOai. 1H-NMR ((CD3)2SO, 300 MHz): delta = 10.03 (s, 1H), 7.79 (t, J = 7.9 Hz, 1H), 7.64-7.57 (m, 3H), 7.54 (t, J = 7.9 Hz, 1H), 7.42 (d, J = 7.9 Hz, 2H), 6.78 (d, J = 8.5 Hz, 2H), 3.71 (s, 6H), 2.43 (sept, J = 6.8 Hz, 2H), 2.29 (sept, J = 6.8 Hz, 2H), 1.27 (d, J = 6.8 Hz, 6H), 1.17 (d, J = 6.8 Hz, 6H), 1.08 (d, J = 6.8 Hz, 6H), 0.99 (d, J = 6.8 Hz, 6H). 13C-NMR ((CD3)2SO, 75 MHz): delta = 158.4, 145.2, 144.7, 139.9, 136.4, 135.2, 133.3, 132.9, 130.2, 129.2, 125.0, 124.8, 104.7, 98.0, 56.9, 28.8, 28.6, 25.8, 23.8, 23.1, 21.7. HR-MS (ESI): Calcd. for C34H44N302 [M+]: 526.3428, found 526.3433.

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-Ethynyl-1,3-dimethoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE REGENTS OF THE UNIVERSITY OF CALIFORNIA; BERTRAND, Guy; GUISADO-BARRIOS, Gregorio; BOUFFARD, Jean; DONNADIEU, Bruno; WO2011/139704; (2011); A2;,
Ether – Wikipedia,
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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. 62257-15-2, name is 2-Fluoro-5-methoxyaniline, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H8FNO

2-Fluoronicotinic acid methyl ester (0.3 g, 1.934 mmol) and 2-fluoro-5-methoxyaniline(0.278 ml, 2.32 1 mmol) were heated by microwave irradiation at 130 C for 20 mm. SomeDCM was added and the mixture was washed twice with 1120. Organic phase was dried overNa2SO4, filtered and evaporated. Crude product was purified by trituration with diethylether. 0.324 g of the title compound was obtained.?H NMR (400 MHz, CDCJ3) oe ppm 3.82 (s, 3 H) 3.95 (s, 3 H) 6.49 (dt, 1 H) 6.78 (dd, I H) 7.03 (dd, I H) 8.27 (dd, I H) 8.33 (dd, I H) 8.42 (dd, 1 H) 10.42 (hr. s., I H).

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; ORION CORPORATION; ARVELA, Riina; HOLM, Patrik; VESALAINEN, Anniina; WO2015/144976; (2015); A1;,
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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. 6346-09-4, name is 4,4-Diethoxybutan-1-amine, A new synthetic method of this compound is introduced below., Application In Synthesis of 4,4-Diethoxybutan-1-amine

To 0.95 g 1-isocyanatonaphthalene (5.62 mmol) dissolved in 20 cm3 of dry benzene 0.90 g 4,4-diethoxybutan-1-amine (5.59 mmol) was added. The mixture was stirred at room temperature for 12 h. The precipitate was filtered off,washed with 10 cm3 benzene, and dried in vacuum(0.01 torr, 4 h, r.t.) to give 6 as white solid. Yield 1.63 g(88%); m.p.: 121-122 C (from ethanol); 1H NMR[600 MHz, (CD3)2SO]: d = 1.11 (6H, t, J = 6.86 Hz,CH3), 1.48-1.52 (2H, m, CH2), 1.56-1.60 (2H, m, CH2),3.14-3.17 (2H, m, CH2), 3.42-3.47 (2H, m, CH2),3.55-3.60 (2H, m, CH2), 4.50 (1H, t, J = 5.49 Hz, CH),6.56 (1H, t, J = 5.48 Hz, NH), 7.41 (1H, t, J = 7.96 Hz,CHAr), 7.49-7.55 (3H, m, CHAr), 7.88 (1H, d,J = 8.23 Hz, CHAr), 7.99 (1H, d, J = 7.68 Hz, CHAr),8.08 (1H, d, J = 8.23 Hz, CHAr), 8.44 (1H, s, NH) ppm;13C NMR [150 MHz, (CD3)2SO]: d = 15.8, 25.6, 31.4,39.5, 61.1, 102.6, 116.9, 121.8, 122.4, 125.8, 126.0, 126.2,126.4, 128.8, 134.2, 135.7, 156.1 ppm; MS (MALDITOF):m/z = 353 ([M+Na]+).

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; Smolobochkin, Andrey V.; Gazizov, Almir S.; Voronina, Julia K.; Burilov, Alexander R.; Pudovik, Michail A.; Monatshefte fur Chemie; vol. 149; 3; (2018); p. 535 – 541;,
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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 437-83-2 as follows. name: 3-Fluoro-2-methoxyaniline

A mixture of 3-fluoro-2-methoxyaniline (1.0 g, 7.1 mmol) and K2CO3 (1.04 g, 7.8 mmol) in DMF (15 mL) was added 1-bromobut-2-yne (981 mg, 7.1 mmol) was stirred at r.t. overnight. The resulting mixture was partitioned between EtOAc and H2O. The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated to give the crude product which was purified by flash chromatography (silica gel, 0-20% EtOAc in PE) to afford the title compound (552 mg, 40% yield) as a yellow oil. LC-MS (ESI): m/z (M+1) = 193.91.

According to the analysis of related databases, 437-83-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; VIIV HEALTHCARE UK LIMITED; JOHNS, Brian Alvin; VELTHUISEN, Emile Johann; WEATHERHEAD, Jason Gordon; (225 pag.)WO2017/93938; (2017); A1;,
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