Tag: M.W=0-100

Electric Literature of 20249-16-5, 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. 20249-16-5, name is 3-Oxocyclobutanecarbonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 59A 3,3-Difluorocyclobutanecarbonitrile Under argon, 14.57 g (153.2 mmol) of 3-oxocyclobutanecarbonitrile from Example 58A were initially charged in 200 ml of absolute dichloromethane, 40.48 ml (306.4 mmol) of diethylaminosulphur trifluoride dissolved in 50 ml of dichloromethane were added at 0 C. and the mixture was stirred at RT overnight. A little at a time, the reaction mixture was then poured into a saturated aqueous sodium bicarbonate solution, cooled to 0 C., and stirred for 30 minutes. The organic phase was separated off and the aqueous phase was extracted with 200 ml of dichloromethane. The combined organic phases were twice washed with water, dried over sodium sulphate, filtered and concentrated. This gave 15.2 g (85% of theory) of the title compound. GC-MS (Method H): Rt=1.43 min MS (ESpos): m/z=98 (M-F)+

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, 3-Oxocyclobutanecarbonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; VAKALOPOULOS, Alexandros; VALOT, Gaelle; FOLLMANN, Markus; WUNDER, Frank; STASCH, Johannes-Peter; MARQUARDT, Tobias; DIETZ, Lisa; LI, Volkhart Min-Jian; RAY, Nicholas Charles; BACHERA, Dominika; (71 pag.)US2017/50961; (2017); A1;,
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Synthetic Route of 630-18-2, 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. 630-18-2 name is Pivalonitrile, 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.

General procedure: To an ice cold solution of pivalonitrile (1f, 120 muL, 1.085 mmol) in Et2O (1.0 mL)was added an ethereal solution of 2-naphthylmagnesium bromide (2b, 0.75 M, 1.88mL, 1.410 mmol) and the reaction mixture was stirred at 60 C in a sealed tube for 2 h.After cooling to 0 C, the reaction mixture was treated with anhydrous MeOH (132muL), followed by the addition of CuBr2 (24.3 mg, 0.109 mmol) and anhydrous DMF(10.0 mL). The resulting reaction mixture was stirred at 80 C under an oxygenatmosphere for 6 h. Then the reaction was quenched by the addition of pH 9ammonium buffer solution and the organic materials were extracted with Et2O. Thecombined organic extracts were washed with water, and then with brine and driedover anhydrous MgSO4. The solvents were removed in vacuo and the resulting crudematerial was purified by flash column chromatography using hexane-EtOAc (90:10)to afford 2-naphthonitrile

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

Reference:
Article; Tnay, Ya Lin; Ang, Gim Yean; Chiba, Shunsuke; Beilstein Journal of Organic Chemistry; vol. 11; (2015); p. 1933 – 1943;,
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Synthetic Route of 6330-25-2, 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. 6330-25-2, name is 2-Cyano-N-methyl-acetamide belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

1.12 g (28.06 mmol) of sodium hydride at 60% in mineral oil are added, fractionwise, to a solution, cooled to 0-5 C., of 1.31 g (13.36 mmol) of N-methylcyanoacetamide (prepared according to 1.3) in 20 ml of anhydrous dimethylformamide. Stirring is continued at this temperature for ten minutes and then a solution of 3.55 g (4.93 mmol) of 6-chloro-2-[(pyridin-2-ylmethyl)amino]nicotinoyl fluoride in 20 ml of dimethylformamide is added. The medium is stirred overnight at ambient temperature and then 0.561 g (14.03 mmol) of sodium hydride at 60% is added fractionwise. Stirring is continued at this temperature for 1 hour minutes, and then the reaction mixture is poured onto ice and the subsequent mixture is acidified to pH 5-6 with an aqueous solution of acetic acid at 10%. The precipitate is isolated by filtration and, after drying in an oven, 3.98 g of the expected product are obtained in the form of a beige solid. MH+=344. Yield=87%. 1H NMR (DMSO-d6, 400 MHz, delta in ppm): delta 9.20 (s, <1H, very broad); 8.85 (s, 1H); 8.30 (m, 1H); 8.10-7.85 (m, 2H, broad); 7.80 (d, 1H); 7.75 (s, 1H, broad); 6.90 (d, 1H); 4.90 (s, 2H); 2.95 (s, 3H). 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-Cyano-N-methyl-acetamide, other downstream synthetic routes, hurry up and to see. Reference:
Patent; SANOFI-AVENTIS; US2010/144757; (2010); 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. 3047-38-9, name is Cyclopent-1-enecarbonitrile, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C6H7N

To a stirred solution of cyclopent- l-enecarbonitrile (50 g, 537 mmol) in carbon tetrachloride (400 ml) at 25C was added N-bromosuccinimide (96 g, 537 mmol) under nitrogen atmosphere. The resulting mixture was refluxed for 2 h. The progress of reaction was monitored by TLC. The reaction mixture was cooled to 25C and filtered through Celite. The filtrate was concentrated under reduced pressure to obtain a crude product, which was purified by column chromatography over silica gel ( 100 – 200 mesh) using 1% ethyl acetate in hexane as an eluent to obtain the title compound (60 g, 65%). iHNMR (CDCls, 400MHz): delta 6.77-6.73 (m, IH), 5. 12-5.09 (m, IH) 2.95-2.86 (m, lH) 2.67-2.42 (m, 3H).

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 3047-38-9.

Reference:
Patent; LUPIN LIMITED; JANA, Gourhari; SINHA, Neelima; KARCHE, Navnath, Popat; KURHADE, Sanjay, Pralhad; TILEKAR, Ajay, Ramchandra; GUPTA, Nishant, Ramniwasji; IRLAPATI, Nageswara, Rao; KUKREJA, Gagan; PALLE, Venkata, P.; KAMBOJ, Rajender, Kumar; (102 pag.)WO2016/12956; (2016); A1;,
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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. 630-18-2, name is Pivalonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: Pivalonitrile

General procedure: To a solution of 4-bromobiphenyl 1a (3.0 mmol, 699.3 mg) in THF (3.0 mL) was added n-BuLi (4.5 mmol, 1.55 M in hexane, 2.87 mL) at 50 C. The obtained mixture was stirred for 30 min at 50 C under an argon atmosphere. Pivalonitrile (6.0 mmol, 498.8 mg) in THF (2.0 mL) was added to the mixture at 50 C and the obtained mixture was stirred for 30 min in the temperature range of 50 C to room temperature. MeOH (2.0 mL) was added to the mixture. Then, I2 (12.0 mmol, 3045.6 mg) and K2CO3 (12.0 mmol, 1658.4 mg) were added to the mixture at room temperature, and the obtained mixture was stirred for 6 h at 70 C. Sat. aq. Na2SO3 solution (20.0 mL) was added to the reaction mixture, and the product was extracted with AcOEt (10.0 mL x 3). The organic layer was dried over Na2SO4. After filtration and removal of the solvent, the residue was purified by silica-gel column chromatography (chloroform: n-hexane 1:1) to give 4-cyanobiphenyl 2a (451.6 mg, 84%).

The synthetic route of 630-18-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Uchida, Ko; Togo, Hideo; Tetrahedron; vol. 75; 39; (2019);,
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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. 6330-25-2, name is 2-Cyano-N-methyl-acetamide, A new synthetic method of this compound is introduced below., SDS of cas: 6330-25-2

0.394 g (9.95 mmol) of sodium hydride at 60% in mineral oil is added, in small amounts, to a solution, cooled to 0-5 C., of 0.483 g (4.93 mmol) of N-methylcyanoacetamide in 7 ml of anhydrous dimethylformamide. Stirring is continued at this temperature for ten minutes and then a solution of 1.0 g (4.93 mmol) of 2-(aminoethyl)-6-chloronicotinic acid fluoride in 5 ml of dimethylformamide is added. The medium is stirred overnight at ambient temperature and then 0.197 g (4.93 mmol) of sodium hydride at 60% is added in small amounts. Stirring is continued at this temperature for 10 minutes and then 0.56 ml (9.78 mmol) of acetic acid is added. 60 ml of water are then added and the solid is spin-filter-dried, rinsed with water, and then dried in an oven. 1.30 g of the expected product are obtained. Melting point: 283-284 C. MH+=281. Yield=94%. 1H NMR (DMSO-d6, 400 MHz): delta 11.75 (s, <1H, very broad); 11.00 (q, 1H, broad); 8.45 (d, 1H); 8.10 (s, 1H broad); 7.40 (d, 1H); 4.40 (q, 2H); 2.80 (d, 3H); 1.25 (t, 3H). The synthetic route of 6330-25-2 has been constantly updated, and we look forward to future research findings. Reference:
Patent; SANOFI-AVENTIS; US2010/144757; (2010); A1;,
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Synthetic Route of 98730-77-9, 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. 98730-77-9 name is 1-(Hydroxymethyl)cyclopropanecarbonitrile, 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.

A mixture of 1-cyanocycloprop-1-ylmethanol (4.31 g, 44.4 mmol), obtained as in the proceeding paragraph, triethylamine (9.04 ml, 64.8 mmol) and methylene chloride (78 ml) was cooled under argon to between 0 and 5C and methanesulfonyl chloride (4.67 ml, 59.9 mmol) was added slowly. The mixture was cooled 3 hours with stirring at 0 to 5C, then diluted with water and extracted with methylene chloride. The extract was washed with 5% sodium bicarbonate, dried (MgSO4) and concentrated to dryness to give 1-cyanocycloprop-1-ylmethyl methanesulfonate.

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

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; EP748800; (1996); A3;,
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Adding a certain compound to certain chemical reactions, such as: 98730-77-9, name is 1-(Hydroxymethyl)cyclopropanecarbonitrile, belongs to nitriles-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 98730-77-9, Computed Properties of C5H7NO

A stirred mixture of 1-(hydroxymethyl)cyclopropanecarbonitrile (24.30mmol, 2.36g) in dichloromethane (3OmL) was treated with triethylamine (48.6mmol, 6.83mL, 4.92g) and portionwise with methanesulfonyl chloride (31.6mmol, 2.445mL, 3.62g) keeping the reaction mixture at O0C. The solution was allowed to stir for 1 hour then diluted with saturated sodium hydrogencarbonate and extracted with 10% methanol/dichloromethane (x3). The organic layers were combined and concentrated under reduced pressure to give the intermediate (i-cyanocyclopropyl)methyl methanesulfonate (3.77g).1H NMR (CDCI3, 400 MHz): delta 1.18 (2H, m), 1.46 (2H, m), 3.14 (3H, s), 4.18 (2H, s)

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; N.V. ORGANON; WO2009/24550; (2009); A1;,
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Reference of 19295-57-9, 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. 19295-57-9, name is 3-Hydroxy-2,2-dimethylpropanenitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 3-hydroxy-2,2-dimethylpropanenitrile (4 g, 40.35 mmol) and CBr4(20.7 g, 62.4 mmol) in anhydrous THF (100 mL) was added a solution of triphenylphosphane(12.7 g, 48.4 mmol) in anhydrous THF (100mL) at 0 C. The reaction mixture was stirred at rtovernight, then the mixture was concentrated in vacuo and the residue was purified by silica gelcolumn chromatography (PE/EtOAc (v/v) = 20/1 ) to give the title product as yellow oil (3.27 g,yield 50.0%). 1HNMR (400 MHz, CDCh) 8 (ppm): 3.40 (s, 2H), 1.47 (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, 3-Hydroxy-2,2-dimethylpropanenitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SUNSHINE LAKE PHARMA CO., LTD.; CALITOR SCIENCES, LLC; DAI, Weilong; XI, Ning; LI, Minxiong; ZHANG, Tao; LI, Xiaobo; HU, Haiyang; CHEN, Wuhong; WANG, Tingjin; LIU, Jun; (188 pag.)WO2017/48675; (2017); A1;,
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Reference of 20249-16-5, These common heterocyclic compound, 20249-16-5, name is 3-Oxocyclobutanecarbonitrile, 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.

into a 500-mL round-bottom flask, was placed a solution of 3-oxocyclobutane-l-carbonitrile (4 g, 42.06 mmol, 1.00 eq.) tetra(propan-2-yloxy)titanium (14.16 g, 62.90 mmol, 1.50 eq.) and 2- methylpropane-2-sulfinamide (6.12 g, 50.49 mmol, 1.20 eq.) in tetrahydrofuran (200 mL). The resulting solution was stirred for 16 hours at 65C. The reaction was cooled to 25C. Then NaBH4 (3.2 g, 84.60 mmol, 2.00 eq.) was added. The mixture was stirred for 2 hours at 25C. The reaction was then quenched by the addition of 200 mL of water. The solids were filtered out and the resulting solution was extracted with ethyl acetate (2×200 mL) and the organic layers were combined. The resulting mixture was washed with brine (2×300 mL), dried over sodium sulfate and concentrated under vacuum. This resulted in 7.2 g (85%) of N-(3- cyanocyclobutyl)-2-methylpropane-2-sulfinamide as a yellow solid.

The synthetic route of 20249-16-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PROTEOSTASIS THERAPEUTICS, INC.; LEE, Po-shun; (180 pag.)WO2017/40606; (2017); A1;,
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