Author: Jessica.F

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. 34667-88-4, name is 2-Fluoro-4-nitrobenzonitrile, A new synthetic method of this compound is introduced below., Formula: C7H3FN2O2

Reference Example 114 4-Amino-2-fluorobenzonitrile To a solution of 2-fluoro-4-nitrobenzonitrile (2.51 g) in methanol (125 mL) was added 10percent palladium carbon (50percent containing water, 237 mg), and the mixture was stirred under a hydrogen atmosphere for 3 hr. The reaction mixture was filtrated, and the filtrate was concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (eluent: hexane-ethyl acetate=1:1) to give the title compound as a pale-yellow solid (yield 1.43 g, 70percent). 1H-NMR (CDCl3)delta: 4.31 (2H, brs), 6.37-6.45 (2H, m), 7.31-7.36 (1H, m).

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; Takeda Pharmaceutical Company Limited; Kajino, Masahiro; Hasuoka, Atsushi; Tarui, Naoki; Takagi, Terufumi; EP2336107; (2015); B1;,
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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. 874-97-5, name is 3-Cyanobenzyl alcohol, A new synthetic method of this compound is introduced below., Application In Synthesis of 3-Cyanobenzyl alcohol

Add p-toluene sulphonic acid (2.11 g, 12.2 mmol) to a solution of 3- hydroxymethyl-benzonitrile( 16.30 g, 122.4 mmol) and 3,4-dihydro-2H-pyran (51.5 g, 612 mmol) in dicliloromethane (500 ml) and stir. After 90 minutes, pour reaction into saturated sodium bicarbonate, remove organics, dry with sodium sulfate, filter and concentrate to give a dark brown oil. Purify the residue by flash chromatography eluting with a gradient of 10-15% ethyl acetate :hexanes to yield the title product as a clear oil (16.20 g, 61%): 1H NMR (CDCl3) delta 1.53-1.91 (m, 6H), 3.56 (m, IH)5 3.88 (m, IH), 4.53 (d, IH), 4.72 (t, IH), 4.81 (d, IH), 7.45 (t, IH), 7.58 (m, 2H), 7.69 (s, IH)

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; ELI LILLY AND COMPANY; WO2006/57860; (2006); A1;,
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134450-56-9, name is 4,5-Difluorophthalonitrile, belongs to nitriles-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. Recommanded Product: 134450-56-9

1.52 g (9.14 mmol) 9H-carbazole and 1.91 g (13.7 mol)of potassium carbonate were placed in a 50-mE recovery flask, and the interior of the flask was substituted with nitrogen. 15 mE of dimethylsulfoxide was added to themixture, which was stirred under a nitrogen stream at room temperature for 1 hout 0.500 g (3.05 mmol) of 4,5-difluo- rophthalonitrile was added to the mixture. The mixture was stirred under a nitrogen stream at room temperature for 3 hours and then at 500 C. for 20 hours. Thereafier, the mixturewas added to water, followed by stirring. The mixture was extracted with toluene. After the extraction, the extracted solution was rinsed with a saturated sodium chlorine aqueous solution. After rinsing, an organic layer and an aqueous layer were separated, and the organic layer was dried byadding magnesium sulfate thereto. After drying, the mixture was suction-filtered to provide a filtrate. The resulting filtrate was concentrated to provide a solid matter, which was purified by silica gel column chromatography. In the purification, a mixed solvent of toluene and hexane (1/4) was firstly used as a developing solvent, then a mixed solvent of toluene and hexane (7/3) was used, and then toluene was used as a developing solvent (the developing ratio was gradually changed). The resulting fraction was concentratedto provide a solid matter, which was then rinsed by reslurrywith a mixed solvent of acetone and methanol, therebyproviding a pale yellow powdered solid matter in a yieldamount of 1.20 g and a yield of 85.8%.

The synthetic route of 134450-56-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KYULUX, INC.; Adachi, Chihaya; Uoyama, Hiroki; Nomura, Hiroko; Goushi, Kenichi; Yasuda, Takuma; Kondo, Ryosuke; Shizu, Katsuyuki; Nakanotani, Hajime; Nishide, Jyunichi; (83 pag.)US9502668; (2016); B2;,
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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. 6575-13-9, name is 2,6-Dimethylbenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C9H9N

General procedure: An oven-dried, three-necked flask was sealed with septa and evacuated/backfilled with N2 three times before starting the reaction. To a mixture of 2.5M n-BuLi in hexane (35 mL, 87.6 mmol) anddry THF (20 mL), maintained at below -70 C, solution of N,N-diethyl-2,4-dimethylbenzamide (10a; 6 g, 29.2 mmol) and 3,4-dimethoxybenzonitrile (11b; 7.15 g, 43.8 mmol) in dry THF (7 mL)were added maintaining the temperature below -60 C. The reaction mixture was stirred at -78 C for 38.5 h. The reaction mixture was then warmed to room temperature and quenched with water. The precipitate was filtered off and washed with water and EtOAc to obtain 9b as an off-white solid. The filtrate was extracted with CH2Cl2, washed with water, and concentrated under reduced pressure. The EtOAc-insoluble fraction was again filtered off and washed with EtOAc to obtain 9b (6.46 g, 74%).

According to the analysis of related databases, 6575-13-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Khadka, Daulat Bikram; Woo, Hyunjung; Yang, Su Hui; Zhao, Chao; Jin, Yifeng; Le, Thanh Nguyen; Kwon, Youngjoo; Cho, Won-Jea; European Journal of Medicinal Chemistry; vol. 92; (2015); p. 583 – 607;,
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Related Products of 6393-40-4, These common heterocyclic compound, 6393-40-4, name is 4-Amino-3-nitrobenzonitrile, 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.

Reference B; Synthesis of 3,4-diaminobenzamidine monohydrochloride; Step 1; A mixture of 4-amino-3-nitrobenzonitrile (63.3 g, 388 mmol) in 1,4-dioxane (600 mL) and anhydrous ethanol (600 mL) was cooled in an ice water bath to 0-5 C and treated with gaseous HCl for 1.5 h. The reaction mixture was tightly sealed and allowed to warm up to room temperature with stirring for 18 h. The flask was then carefully unsealed and the reaction mixture was diluted with anhydrous diethyl ether (about 2.4 L) until a cloudy solution was obtained. A minimum amount of absolute ethanol required to give a clear solution was then added, and the resulting solution stirred until crystals of 4-amino-3-nitro-benzimidic acid ethyl ester were observed. Ether was then cautiously added to complete the crystallization process and the suspension was allowed to stand for about 30 minutes. The crystals were filtered and washed with dry diethyl ether, then allowed to dry under aspirator vacuum. The crystals were dried in vacuo to give 4-amino-3-nitro-benzimidic acid ethyl ester hydrochloride (84.6 g) as off-white crystals.

The synthetic route of 6393-40-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AXYS PHARMACEUTICALS, INC.; WO2005/118554; (2005); A2;,
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Related Products of 1080-74-6, A common heterocyclic compound, 1080-74-6, name is 2-(3-Oxo-2,3-dihydro-1H-inden-1-ylidene)malononitrile, molecular formula is C12H6N2O, 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.

General procedure: Compound III (150 mg, 0.16 mmol) and malononitrile(43 mg, 0.65 mmol) were dissolved in CHCl3 (30 mL), then 3 drops ofpiperidine were added. The mixed solution was degassed for 10 min bybubbling nitrogen. The reaction solution was heated at 65 C for 10 h.After completing, the solution was cooled to room temperature. Thesolvent was removed, and the solid crude product was obtained bymethanol precipitation. The crude product was purified by silica gelcolumn chromatography by using CHCl3 as the eluent to obtain a darkredsolid (122 mg, 74%).

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; Zhang, Tong; Yu, Tianzhi; Zhao, Yuling; Wei, Chengjin; Ma, Hailin; Li, Yanmei; Zhang, Hui; Dyes and Pigments; vol. 177; (2020);,
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Reference of 16532-79-9, 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. 16532-79-9, name is 4-Bromophenylacetonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 2: Preparation of l-(4-bromophenyl)cyclopropanecarbonitrile; To a room temperature solution of 4-bromophenylacetonitrile ( 18.0 g) in a solution of 22 mL of sodium hydroxide (50% in water WAV) were added l-bromo-2-chloroethane and (12.0 mL) and benzyltriethylammonium chloride (627 mg). The mixture was heated at 600C overnight. The reaction mixture was cooled to room temperature and diethyl ether was added (300 mL) and partitioned. The ether layer was washed with water (100 mL), hydrogen chloride (100 mL, 10% HCl in water), brine and dried with magnesium sulfate. Upon removal of the solvent in vacuo, the residue was purified by swish using diethyl ether and hexanes to yield the title compound.1H NMR (CD3COCD3) delta 7.60 (2 H, d), 7.35 (2 H, d), 1.74-1.80 (2 H, m), 1.52-1.57 (2 H, m).

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

Reference:
Patent; MERCK FROSST CANADA LTD.; WO2006/133559; (2006); A1;,
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Electric Literature of 58633-04-8, 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. 58633-04-8, name is 4-Amino-3,5-dibromobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 2 Preparation of 3,5-Dibromobenzonitrile STR16 To a stirred solution of t-butylnitrite (53.5 muL, 0.449 mmoles) in 1 ml sieve dried dimethylformamide at 50 C. under an atmosphere of nitrogen was added a solution of 4-amino-3,5-dibromobenzonitrile (50 mg, 0.179 mmoles) in 1 mL of DMF. The mixture was stirred at 50 C. for 0.5 hour and partitioned between diethyl ether, ice-water, and ammonium chloride. The organic phase was separated, washed with water and brine, dried over anhydrous sodium, filtered, and evaporated. Purification by plate layer chromatography using hexane-ethyl acetate (9:1) as eluant provided 28 mg (59%) of white, crystalline product. NMR(CDCl3) delta: 7.7 (d, J=1.8Hz, 2H), 7.9 (t, J=1.8Hz, 1H).

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, 4-Amino-3,5-dibromobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Merck & Co., Inc.; US5192758; (1993); A;,
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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. 75279-53-7, name is 4-Chloro-2-fluorobenzeneacetonitrile, A new synthetic method of this compound is introduced below., SDS of cas: 75279-53-7

Intermediate 36: tert-Butyl 4-((4-chloro-2-fluorophenyl)(cyano)methyl)piperidine-1-carboxylate A solution of 2-(4-chloro-2-fluorophenyl)acetonitrile (0.353 g, 2.082 mmol) in DMF (5 mL) was cooled to 0-5 C., to this was added sodium hydride (0.050 g, 2.082 mmol) and tert-butyl 4-bromopiperidine-1-carboxylate (0.5 g, 1.893 mmol). The reaction was stirred at room temperature for 3 hours. The mixture was quenched with ice/water and partitioned between ethyl acetate and water. The phases were separated and the aqueous extracted with ethyl acetate. The combined organics were washed with water, dried (Na2SO4) and concentrated in vacuo. The crude product was purified by column chromatography on silica, eluted with 0-50% ethyl acetate/petroleum ether to afford ten-butyl 4-((4-chloro-2-fluorophenyl)(cyano)methyl)piperidine-1-carboxylate (0.5 g, 75%).

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; Carroll, Colm; Goldby, Anne; Teall, Martin; US2013/324576; (2013); A1;,
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Adding a certain compound to certain chemical reactions, such as: 1897-52-5, name is 2,6-Difluorobenzonitrile, 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 1897-52-5, Formula: C7H3F2N

General procedure: To an oven dried round bottom flask charged with a mixture of 2-fluorobenzonitrile (1a, 1 mmol) and hydrazine (2a, 1mmol) in ethanol (3 ml), stirred the reaction mixture at 80 C, for 30 min. To the reaction mixture isatin (3a, 1 mmol), 5,5-dimethyl-1,3-cyclohexanedione (4a, 1 mmol) and p-TSA (40 mol %) was added and the reaction mixture was further stirred at 80 C for 4 h. The progress of the reaction was monitored by TLC. After completion of the reaction, solid products was filtered under vacuum, air dried, to obtain the analytically pure products. The compounds 5a-5r were also synthesized by adopting this procedure.

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, 2,6-Difluorobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Balwe, Sandip Gangadhar; Lim, Kwon Taek; Cho, Byung Gwon; Jeong, Yeon Tae; Synthetic Communications; vol. 49; 4; (2019); p. 602 – 610;,
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