Tag: M.W=0-100

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. 4475-95-0, name is 2-Amino-2-methylbutanenitrile, A new synthetic method of this compound is introduced below., SDS of cas: 4475-95-0

5:00 g (50.94 mmol) of 2-amino-2-methylbutanonitril [synthesis described in: Lonza AG, US 5,698,704 (1997);Deng, SL et al.Synthesis 2001, 2445;Hjorringgaard, CU et al.. J. Org. Chem 2009, 74, 1329;Ogrel, A. et al.EUR. J. Org. Chem. 2000, 857] were introduced into 50 ml of THF and 6.5 ml of water, 21.83 g (157.92 mmol) of potassium carbonate and treated at 0 C slowly with 7.9 ml (56.04 mmol) Benzylchlorocarbonat (benzylchloroformate) ,After addition of 8 ml THF and 3 ml of water, the reaction mixture was stirred slowly at RT coming overnight.Then was treated with water and extracted three times with ethyl acetate.The combined organic phases were dried over sodium sulfate and concentrated.The residue was dissolved in diethyl ether and precipitated with petroleum ether.The product was filtered off, the solid washed with a little petroleum ether and dried under high vacuum.There were 11:35 g of the target compound (93%. Th.)

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.

Application of 4426-11-3, 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. 4426-11-3, name is Cyclobutanecarbonitrile, This compound has unique chemical properties. The synthetic route is as follows.

(a) A solution of borane-tetrahydrofuran complex [(1M] in tetrahydrofuran, [120ML)] was added over [10MIN] to a solution of cyclobutane carbonitrile (8. [1G)] [Lancaster] in dry tetrahydrofuran [(20ML)] under nitrogen at room temperature. The solution was refluxed overnight then cooled to [20.] Methanol [(150ML)] was added dropwise over 15mins keeping the temperature below [25,] then the mixture was cooled to [0 AND] dry hydrogen chloride was bubbled through for 30min. The resulting mixture was refluxed for 90min, evaporated and the residue re-evaporated twice from methanol. Ether [(150ML)] was added and the resulting solid was filtered off. It was taken up in hot isopropanol [(50ML),] filtered, and hot acetonitrile [(30ML)] added. The mixture was cooled and the solid filtered off to give the [C-CYCLOBUTYLMETHYLAMINE] hydrochloride (5.7g) NMR (400 MHz, DMSO-d6) F6382 1.8 (4H, m), 2.0 (2H, m), 2.54 [(1H,] m), 2.80 (2H, d), 8.0 (3H, [BR S).]

The chemical industry reduces the impact on the environment during synthesis Cyclobutanecarbonitrile. I believe this compound will play a more active role in future production and life.

Related Products of 3047-38-9, 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. 3047-38-9 name is Cyclopent-1-enecarbonitrile, 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.

Step 1: 3-bromocyclopent-1-enecarbonitrile To a stirred solution of cyclopent-1-enecarbonitrile (50 g, 537 mmol) in tetrachloromethane (400 ml) at 25 C. was added 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 cooled to 25 C. 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%). 1HNMR (CDCl3, 400 MHz): delta 6.77-6.73 (m, H), 5.12-5.09 (m, 1H) 2.95-2.86 (m, 1H) 2.67-2.42 (m, 3H)

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

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. 105-34-0, name is Methyl 2-cyanoacetate, A new synthetic method of this compound is introduced below., name: Methyl 2-cyanoacetate

1-nitro-naphthalene (97 g, 0.56 mol), methyl cyanoacetate (166.5 g, 1.68 mol), potassium cyanide (40.1 g, 0.62mol), potassium hydroxide (62.9 g, 1.12 mol) and dissolved in dimethylformamide (970 mL) and the mixture was stirred overnight at 60C. After concentrated under reduced pressure to remove the solvent at room temperature into a 500 mL 10% aqueous sodium hydroxide solution was refluxed for about one hour. After extraction with ethyl acetate and separated by column chromatography and recrystallized from toluene-heptane to give the Sub 2-2-1 50.8 g (yield: 54%).

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.

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. 2469-99-0, name is 3-Oxobutanenitrile, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 3-Oxobutanenitrile

To a stirred solution of 3oxobutanenitriie (10.00 g, 120.00 mrnol) in DMF (30 mL) was added DMF-DMA (1934 mL, 144.00 rnrnoi) and the reaction mixture was stirred at 80 0Q for 16 h. The reaction mixture was cooled to ambient temperature, concentrated to dryness and diluted with nhexane (200 rnL), The precipitate was collected by suction filtration and dried undervacuum to obtain Intermediate 41A (1300 g, 78.00%). ?H NMR (400 MHz, DMSOd6) pprn2.17 (s, 3 H), 3.25 (s, 3 H), 3.29 (s, 3 H), 7.83 (s, I H). LCMS (Method-L): retention time 054 miii, [M+i-I] 139.2.

According to the analysis of related databases, 2469-99-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; GUNAGA, Prashantha; BHIDE, Rajeev S.; BORA, Rajesh Onkardas; PANDA, Manoranjan; YADAV, Navnath Dnyanoba; PRIESTLEY, Eldon Scott; RICHTER, Jeremy; (321 pag.)WO2018/93569; (2018); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Application of 98730-77-9,Some common heterocyclic compound, 98730-77-9, name is 1-(Hydroxymethyl)cyclopropanecarbonitrile, molecular formula is C5H7NO, 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.

Thionyl chloride (1.6 mL) was added to a solution of 1-(hydroxymethyl)cyclopropanecarbonitrile (1.42 g) in toluene (20 mL) at room temperature. The reaction mixture was stirred at 80C for 2 hr, and the solvent was evaporated. The resulting residue was dissolved in DMF (20 mL), and 2-bromo-5-(4-hydroxy-3-methoxyphenyl)furo[3,2-c]pyridin-4(5H)-one (2.45 g) and potassium carbonate (4.03 g) were added. The mixture was stirred at 80C overnight. To the reaction mixture was added saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate three times. The resulting organic layer was dried over magnesium sulfate and concentrated in vacuo, and the resulting residue was filtered through NH silica gel. The filtrate was concentrated in vacuo, and the resulting solid was washed with IPE to give the title compound (2.80 g) as a white solid. MS (ESI+):[M+H]+ 416.1.

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

Reference:
Patent; Takeda Pharmaceutical Company Limited; KASAI, Shizuo; IGAWA, Hideyuki; TAKAHASHI, Masashi; KINA, Asato; EP2848622; (2015); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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. 630-18-2, name is Pivalonitrile, A new synthetic method of this compound is introduced below., category: nitriles-buliding-blocks

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);,
Nitrile – Wikipedia,
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Synthetic Route of 630-18-2,Some common heterocyclic compound, 630-18-2, name is Pivalonitrile, molecular formula is C5H9N, 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.

The title compound is prepared from commercially available materials by those skilled in the art by adaptation of a patent reference (Neighbors et al, US 3,547,621).To a solution of hydroxylamine hydrochloride (6.80 g, 97.9 mmol) in water (15 mL) is added slowly a solution of potassium carbonate (6.15 g, 44.5 mmol) in water (10 mL) and 2,2- dimethyl propionitrile (6.25 g, 89.0 mmol) in ethanol (50 mL). The mixture is stirred at room temperature for 30 min then heated at reflux for 16 h. After this time, dichloromethane (75 mL) and water (50 mL) are added and the aqueous layer is extracted with dichloromethane (3 x 50 mL). The organic layers are combined, washed with brine (20 mL), dried (Na2SO4), filtered and concentrated under reduced pressure to afford the title compound as a white solid (6.15 g, 60%). 1H NMR (400 MHz, CHLOROFORM-d) delta ppm 1.21 (9 H, s), 4.57 (2 H, br. s.), 9.15 (1 H, br. s.).

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

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BOEHRINGER INGELHEIM PHARMA GMBH & CO. KG; WO2009/140089; (2009); A2;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Application of 6330-25-2, These common heterocyclic compound, 6330-25-2, name is 2-Cyano-N-methyl-acetamide, 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.

N -Methyl 2-amino-5-(2-(4-methoxyphenyl)ethyl)thiophene-3-carboxamide (TJ19). To a mixture of 4-(4-methoxyphenyl)butanal 6 (0.5 g, 2.805 mmol), 2-cyano-N- methylacetamide 8 (0.275 g, 2.805 mmol) and sulfur (0.090g, 2.805 mmol) in DMF (10 mL), NEt3(0.851 g, 8.451 mmol, 3 equiv) was added. After stirring the resulting mixture at 60C for 30 hrs, the reaction mixture was added to water (20 mL). Ethyl acetate (20 mL) was added and the organic solution was washed with distilled water (3 chi 20 mL), dried over MgS04, filtered, and then evaporated to dryness to afford the crude product mixture. Purification by column chromatography (silica, eluent CH2CI2- ethyl acetate 90-10) afforded TJ19 (0.27 g, 33%) as an off-white solid. 1H NMR (300 MHz, CDCI3) deltaEta 2.86 (m, 7H); 3.78(s, 3H); 5.57 (s, 2H); 6.64(s, 1 H); 6.81 (d, 2H); 7.06(d, 2H).

Statistics shows that 2-Cyano-N-methyl-acetamide is playing an increasingly important role. we look forward to future research findings about 6330-25-2.

Reference:
Patent; KATHOLIEKE UNIVERSITEIT LEUVEN; UNIVERSITA DEGLI STUDI DI FERRARA; BALZARINI, Jan; DEHAEN, Wim; THOMAS, Joice; LIEKENS, Sandra; ROMAGNOLI, Romeo; BARALDI, Pier Giovanni; WO2013/190137; (2013); A2;,
Nitrile – Wikipedia,
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Related Products of 2469-99-0,Some common heterocyclic compound, 2469-99-0, name is 3-Oxobutanenitrile, molecular formula is C4H5NO, 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.

Weighing 0.22 muM of sodium cyanide (2.2 equiv) in 250 ml three-neck bottle in, under ice bath by adding 110 ml THF, then adding 0.1 muM 1 a (1 equiv) and 0.1 muM 1 d (1 equiv), 65 C reflow 12 h. After the reaction, under the ice, with a certain amount of reaction water quenching, adjusting solution PH value to 4 – 5, ethyl acetate extraction, the organic phase is dried with anhydrous sodium sulfate, and steaming and get products 2 ad. 250 Ml three-neck bottle is added to the product of the 1st step 2 ad, 100 ml ethanol and 0.9 muM 2 g, 85 C reflow 18 h. Stopping the reaction, steaming and out ethanol, saturated sodium hydroxide solution to adjust the residue for the PH in 9 – 10. DCM extraction, the organic phase is dried with anhydrous sodium sulfate, and steaming and, column chromatography purification (dichloromethane: ethyl acetate=20:1) to obtain the product B3.

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

Reference:
Patent; China Agricultural University; Hou Shicong; Gao Gui; Chen Xiangzhu; Liu Jingjing; Zhang Yuanyuan; Zhang Xueyan; (10 pag.)CN107980784; (2018); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts