Month: March 2021

Reference of 150-78-7, The chemical industry reduces the impact on the environment during synthesis 150-78-7, name is 1,4-Dimethoxybenzene, I believe this compound will play a more active role in future production and life.

EXAMPLE 61 (+,-)-N-(cis-2-(3,6-dimethoxy-2-fluorophenyl)-cyclopropyl)-N’-(5-chloropyrid-2-yl)-urea To a solution of 1,4-dimethoxybenzene (15.0 g, 0.109 mol) in 300 mL of dry THF was added 2.5M n-butyllithium (45.6 mL, 0.114 mol) at room temperature under nitrogen. After addition was complete, the solution was stirred for 1 hr. The mixture was cooled to -70 C. and N-fluorobenzenesulfonimide (36.0 g, 0.114 mol) in 150 mL of THF was added slowly, keeping the temperature below -60 C. The solution was allowed to warm to room temperature during the night. 100 mL of NH4 Cl (sat) was added and the mixture was extracted with diethyl ether/THF. The organic phase was washed with 1M NaOH (2*60 mL), dried over MgSO4 and evaporated. Column chromatography (silica gel, n-hexane followed by 1, 5 and 10% EtOAc in n-hexane) provided 11.43 g of a mixture of 1,4-dimethoxy-2-fluorobenzene and 1,4-dimethoxybenzene (4.3:1). This mixture was reacted in a manner analogous to Examples 362, 375 and 348 of WO 93/03022 to give (+,-)-cis-2-(3,6-dimethoxy2-fluorophenyl) cyclopropylamine.

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, 1,4-Dimethoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Medivir AB; US5849769; (1998); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

These common heterocyclic compound, 5397-31-9, name is 3-((2-Ethylhexyl)oxy)propan-1-amine, 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. COA of Formula: C11H25NO

c) 19.9 parts of the trisazo dyestuffs of part b) above are suspended in 100 parts of water, 10.0 parts of [DIPROPYLENE] glycol monomethyl ether and 4. [8] parts of sodium acetate. After warming at [96C] for over one hour, 5.9 parts of copper sulphate are added in small portions for over one hour, followed by 20.0 parts of 25% ammonia. The mixture is heated to reflux for 12 hours whereupon a voluminous suspension of the copper complex results. The temperature is allowed to fall to [45C] over 2 hours (while stirring well) and the suspension is slowly reacted with a solution of 13.3 parts of [3-[(2-ETHYLHEXYL) OXY]-1-] propanamine in 70 parts of water and [8.] 3 parts of 30% HCI. The resulting precipitate is stirred a further hour at room temperature, filtered and the residue is washed salt free and dried. A compound of formula wherein R is methoxy, is obtained.

The synthetic route of 3-((2-Ethylhexyl)oxy)propan-1-amine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CLARIANT INTERNATIONAL LTD; WO2003/99937; (2003); A1;,
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. 1836-62-0, name is 2-(2-Methoxyphenoxy)ethylamine, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 1836-62-0

Example 1 Preparation of Carvedilol in Neat Conditions 2-(2-Methoxyphenoxy)ethylamine (III) (4.89 g) was heated to about 100 C., after which 4-(oxiran-2-ylmethoxy)-9H-carbazole (II) (3.31 g) was added portionwise. After approximately 20 minutes, the reaction mixture was cooled to about 70 C., after which water (25 ml) and ethyl acetate (15 ml) were added. The pH of the two-phase mixture was then adjusted to 5 with 2 N hydrochloric acid. The solid that formed, Carvedilol hydrochloride hydrate, is filtered, washed with water (20 ml) followed with ethylacetate (15 ml). The resulting material is reslurried in ethylacetate (50 ml) and water (20 ml) containing 5% Sodium carbonate until the pH reached 7.5. The organic phase was separated and dried over sodium sulfate. The dried solution was concentrated to a turbid solution and cooled overnight to about 4 C. Precipitated carvedilol was isolated by filteration and crystallized from isopropanol.

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 1836-62-0.

Reference:
Patent; Hildesheim, Jean; Finogueev, Sergey; Aronhime, Judith; Dolitzky, Ben-Zion; Ben-Valid, Shoshana; Kor, Ilan; US2002/143045; (2002); A1;,
Ether – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 20781-20-8, name is (2,4-Dimethoxyphenyl)methanamine, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 20781-20-8, Safety of (2,4-Dimethoxyphenyl)methanamine

a. Potassium carbonate (2.97 g, 21.5 mmol) was added to a mixture of 2- chloropyrimidine (2.1 g, 17.9 mmol), 2,4-dimethoxybenzylamine (3.0 g, 17.9 mmol) and acetonitrile (20 mL). The reaction mixture was heated at reflux for 16 h, allowed to cool to ambient temperature and partitioned between ethyl acetate (150 mL) and water (10 mL). The organic phase was washed with water (2 10 mL) and brine (10 mL), dried over anhydrous sodium sulphate, filtered and concentrated in vacuo. The residue was triturated in diethyl ether (20 mL), washed with hexanes (20 mL) and purified by column chromatography, eluting with a 0-100% gradient of ethyl acetate in hexanes to afford A/-(2,4-dimethoxybenzyl)pyrimidin-2-amine as a pale yellow solid in 84% yield (3.70 g): MS (ES+) m/z 245.9 (M + 1).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, (2,4-Dimethoxyphenyl)methanamine, and friends who are interested can also refer to it.

Reference:
Patent; XENON PHARMACEUTICALS INC.; LIU, Shifeng; FOCKEN, Thilo; CHAHAL, Navjot; ZHANG, Zaihui; OBALLA, Renata, Marcella; FONAREV, Julia; WO2013/64984; (2013); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 29578-83-4, name is 1-Bromo-3-methoxy-5-methylbenzene, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 29578-83-4, COA of Formula: C8H9BrO

A mixture of NBS (5.31 g, 29.83 mmol, 1.20 equiv), AIBN (2.04 g, 12.42 mmol, 0.50 equiv), Cd4 (100 mL), and 1-bromo-3-methoxy-5-methylbenzene (5.00 g, 24.87 mmol, 1.00 equiv) was stirred for 12 h at 80C under nitrogen. The reaction was then quenched by water, extracted with dichloromethane, washed with brine, dried over anhydrous sodium sulfate, and concentrated under vacuum. The residue was purified by a silica gel column eluting with ethyl acetate/petroleum ether (1:100) to afford the title compound (6 g, 86%) as a light yellow solid.

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, 1-Bromo-3-methoxy-5-methylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; GENENTECH, INC.; CHEN, Huifen; CHU, Yanyan; DO, Steven; ESTRADA, Anthony; HU, Baihua; KOLESNIKOV, Aleksandr; LIN, Xingyu; LYSSIKATOS, Joseph P.; SHORE, Daniel; VERMA, Vishal; WANG, Lan; WU, Guosheng; YUEN, Po-wai; WO2015/52264; (2015); A1;,
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 31804-36-1 as follows. category: ethers-buliding-blocks

(E)-ethyl 3-(3-methoxy-2-methylphenyl)acrylateTo a solution of 1-bromo-3-methoxy-2-methylbenzene (515 mg, 2.56 mmol) in DMF (10 ml_) at RT was added ethyl acrylate (2564 mg, 25.6 mmol) and N-ethyl-N- isopropylpropan-2-amine (2.68 ml_, 15.37 mmol), tri-o-tolylphosphine (312 mg, 1.025 mmol), Pd(OAc)2(1 15 mg, 0.512 mmol). The reaction mixture was heated in microwave under high absorption at 150 C for 2 h. The reaction mixture was passed through celite and washed with EtOAc. The filtrate was washed with water twice, brine (1x). The organic layer was collected and concentrated to give the crude product. The crude product was purified on a silica cartridge (40 g) with a Combiflash Companion, eluting at 35 mL/min with a gradient running from 0 % EtOAc/hexanes to 50 % over 35 min. The desired fractions were concentrated under reduced pressure to give 450 mg (80 %) of the title compound. LC-MS m/z 220.9 (M+H)+, 1.11 (ret. time).

According to the analysis of related databases, 31804-36-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; ASTEX THERAPEUTICS LIMITED; BOEHM, Jeffrey Charles; DAVIES, Thomas Glanmor; WOOLFORD, Alison Jo-anne; GRIFFITHS-JONES, Charlotte Mary; WILLEMS, Hendrika Maria Gerarda; NORTON, David; SAXTY, Gordon; HEIGHTMAN, Thomas Daniel; LI, Tindy; KERNS, Jeffrey K.; DAVIS, Roderick S.; YAN, Hongxing; WO2015/92713; (2015); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 36865-41-5, name is 1-Bromo-3-methoxypropane, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 36865-41-5, Formula: C4H9BrO

To a suspension of Mg (911 mg, 37.5 mmol) and of iodine (one crystal) in dry THF (30 mL) was added dropwise 5% of the total amount of 1-bromo-3-methoxypropane (4.59 g, 30.0 mmol). The mixture was heated to reflux with the help of a heat gun until the Grignard formation had started. The rest of the 1-bromo-3-methoxypropane was added slowly, while an exothermic reaction proceeded. After the end of the addition, the reaction mixture was stirred under reflux for 20 min, and was allowed to cool to rt. This Grignard sol. (1M in THF, 23.5 mL, 23.5 mmol) was added dropwise to a mixture of 2-bromo-5-chloro-4-dimethoxymethyl-pyridine (2.50 g, 9.38 mmol) and Ni(dppp)Cl2 (495 mg, 0.938 mmol) in THF (50 mL) at 0 C. The reaction mixture was stirred at rt for 30 min, and was then heated to reflux for 2 h. The mixture was allowed to cool to rt, and was dissolved with EtOAc. This mixture was washed with aq. sat. NaHCO3. The org. layer was dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the residue by FC (heptane?EtOAc/heptane 1:1) yielded the title compound (1.51 g, 62%). LC-MS: tR=0.80 min; ES+: 260.15.

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

Reference:
Patent; Actelion Pharmaceuticals Ltd.; US2009/62342; (2009); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Related Products of 910251-11-5, 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 910251-11-5 as follows.

To a solution of 208A (300mg, O.lmmol) and potassium trifluoro(methoxymethyl)borate (304mg, 0.2 mmol) in 3 ml dioxane/water (10:1) was added 3 aq. Cs2C03 and 2- dicyclohexylphosphino-2′,6′-diisopropoxybiphenyl (Ruphos)(93.4mg, 0.2 mmol) andPalladium(II)acetate (22.5 mg, 0.1 mmol). The resulting mixture was heated at reflux for overnight. The reaction mixture was filtered and the mixture was extracted with EtOAc. The organics were dried over Na2S04, filtered and concentrated. The crude product was purified by Si02 chromatography eluting with a gradient of EtOAc in hexanes to provide 12 mg of title compound. MS (m/z) 267 [M+H]+.

According to the analysis of related databases, 910251-11-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GILEAD SCIENCES, INC.; BONDY, Steven S.; CANNIZZARO, Carina E.; CHOU, Chien-hung; HALCOMB, Randall L.; HU, Yunfeng Eric; LINK, John O.; LIU, Qi; SCHROEDER, Scott D.; TSE, Winston C.; ZHANG, Jennifer R.; WO2013/6738; (2013); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 10541-78-3, name is 2-Methoxy-N-methylaniline, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 10541-78-3, Quality Control of 2-Methoxy-N-methylaniline

This compound was obtained by reacting 2-methoxy-N-methylaniline (3.0 g, 21.9 mmol.) and cyclopentanone (9.20 g, 109mmol) in the presence of a catalytic amount of iodine (278 mg, 1.09 mmol).After purification on a silica gel column using hexanes-ethyl acetate (95: 5),compound 10a was obtained as a yellowish oil (2.35 g, 42%). 1H NMR (CDCl3, 400 MHz): delta 1.68-1.72(2H, m), 1.76-1.82 (2H, m), 1.85-1.92 (2H, m), 2.01-2.07 (2H, m), 2.51-2.56(2H, m),2.65-2.70 (2H, m), 4.05 (3H, s), 4.47 (1H, brs, NH), 5.01 (1H, m), 6.03(1H, m), 6.58 (1H, d, J = 7.6 Hz),6.60 (1H, d, J = 4.0 Hz), 6.65 (1H,dd, J = 7.6 and 4.0 Hz). 13CNMR (CDCl3, 100 MHz): delta 22.6, 24.1, 31.6, 32.4, 40.2, 55.8, 64.8,109.3, 115.9, 116.3, 120.5, 132.2, 132.3, 138.8, 145.4. EI-MS (GC-MS): m/z(5) 255 [M]+ (30), 227(100), 213(15)

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-Methoxy-N-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Fotie, Jean; Ayer, Suraj K.; Poudel, Binit S.; Reid, Carolyn S.; Tetrahedron Letters; vol. 54; 51; (2013); p. 7069 – 7073;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Application of 1579-40-4, The chemical industry reduces the impact on the environment during synthesis 1579-40-4, name is Di-p-tolyl Ether, I believe this compound will play a more active role in future production and life.

Tolyl Ether (5.9 gm, 30 mmoles), bipheylcarboxylic acid (6 gm, 30.27 mmoles), zinc chloride (12 gm, 88 mmoles) and phosphorus oxychloride (20 mmoles) were stirred at 95 degree in an oil bath for 2 hrs. The mixture was cooled to room temperature and the viscous mixture is poured into cracked ice and stirred overnight. The solid was collected and washed with water. The solid was suspended in 150 ml of methanol and was heated to boiling for 5 min. The mixture was cooled to room temperature, filtered and dried to a constant weight (8.4 g, yield: 74%).

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, Di-p-tolyl Ether, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ISIS PHARMACEUTICALS, INC.; WO2005/77966; (2005); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem