Tag: M.W=100-200

Adding a certain compound to certain chemical reactions, such as: 37719-02-1, name is 2,2-Dimethyl-3-oxobutanenitrile, 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 37719-02-1, name: 2,2-Dimethyl-3-oxobutanenitrile

The effects of temperature on KH for Examples 2-6 to 2-11 were measured using Technique 2 and are listed in Table 2. The van’t Hoff equation was then fit to a plot of KH vs. temperature; energy standard deviation were calculated from the fit of the equation to the raw data. (0078) Examples 2-6 and 2-11 were prepared using variations to the standard procedure. Example 2-6 was prepared with a concentration of 50 mM, so that it was soluble in water. For Example 2-11, a small amount of enol was also observed (about 0.08 relative to ketone). To account for this, we calculated KH for Example 2-11 as diol/(ketone+enol), assuming enol formation from the ketone is reversible.

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, 2,2-Dimethyl-3-oxobutanenitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; University of Pittsburgh – Of the Commonwealth System of Higher Education; Beckman, Eric J.; Bourmpakis, Ioannis; Tavenor, Nathan Albert; (18 pag.)US2020/78703; (2020); A1;,
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Reference of 74231-65-5, The chemical industry reduces the impact on the environment during synthesis 74231-65-5, name is 4-(Dichloromethyl)benzonitrile, I believe this compound will play a more active role in future production and life.

Under argon protection,Add 400 mL dioxane to a 2 L round bottomed flaskwithCyano dichlorobenzene 55g,The mixture was cooled to -30 C,Then slowly added dropwise 200mL,1mol / L dimethyl zinc n-hexane solution.Bi completed,The reaction was stirred at this temperature for 2 hours,A large number of reaction bottle appeared brown precipitate,For p-cyanodimethylzinc complex.Weigh 146g of triphenylphosphine ruthenium dichloride,With 180mL dissolved in dioxane was added to the reaction,The reaction was stirred at -20 C for 2 hours.Weigh tricyclohexyl phosphine 136g,Dissolved in 160mL dioxane was added to the reaction flask,The reaction was stirred for 1 hour,A purple solution.Most of the solvent and the volatile matter were distilled off under reduced pressure,The residue was recrystallized from 800 mL of methanol for 1 hour at room temperature,Get a lot of brown red product,filter,The solid was washed several times with methanol,Vacuum drying provided catalyst precursor 1 (89 g,Yield 71%)

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-(Dichloromethyl)benzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Zhongyou Haike Ranqi Co., Ltd.; Shanghai Chemical Institute Co., Ltd.; Luo Yong; Ping Jian; Wang Yuan; Shen Kaimin; Yang Weicheng; Chen Fuxiang; Fang Chao; (9 pag.)CN107216355; (2017); A;,
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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 159847-80-0 as follows. category: nitriles-buliding-blocks

4-Amino-3-cyano-benzoic acid methyl ester (1.4 g, 7.95 mmol) was dissolved in a mixed solution of tetrahydrofuran and methanol (1/1, 50 mL), and iodine (I2, 2.2 g, 8.74 mmol) and silver nitrate (AgNO3, 1.5 g, 8.74 mmol) were added dropwise thereto. The mixture was stirred for 6 hours at room temperature and filtered with celite. The filtrate was added with 10% sodium thiosulfate aqueous solution and extracted with ethyl acetate. The extract was washed with brine, dried with anhydrous magnesium sulfate and filtered. The filtrate was distilled under reduced pressure. The residue was separated by column chromatography to obtain the title compound (2.0 g, 84%).

According to the analysis of related databases, 159847-80-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; LG LIFE SCIENCES LTD.; PAEK, Seung Yup; LEE, Sung Bae; PARK, Deok Seong; LEE, Won Hyung; WO2014/129796; (2014); A1;,
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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. 508203-48-3, name is 2,3-Difluoro-4-methylbenzonitrile, A new synthetic method of this compound is introduced below., category: nitriles-buliding-blocks

To a suspension of 2,3-difluoro-4-methylbenzonitrile (5.0 g, 32.6 mmol) in ethanol (1 1 1 mL) at 25C was added hydroxylamine hydrochloride (4.5 g, 65.3 mmol). The reaction mixture was heated at 30 80C for 2 hours. After allowing the reaction to reach room temperature the volatiles were removed under reduced pressure thus affording a white solid that was used in the next step without purification. (0450) NMR (400 MHz, CDCI3) delta ppm: 7.30 (m, 1 H), 6.95 (m, 1 H), 6.50 (brs, 1 H), 5.05 (brs, 2H), 2.30 (s, 3H).

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; SYNGENTA PARTICIPATIONS AG; HOFFMAN, Thomas, James; STIERLI, Daniel; BEAUDEGNIES, Renaud; POULIOT, Martin; HAAS, Ulrich, Johannes; (101 pag.)WO2018/177880; (2018); A1;,
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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. 6476-32-0, name is 2-Phenoxybenzonitrile, A new synthetic method of this compound is introduced below., COA of Formula: C13H9NO

A solution of 2-phenoxybenzonitrile (from step (ii) above (10.1 g, 0.0517 mol) in THF (50 ml) was added dropwise to the well-stirred suspension of LAH (4.9 g, 0.129 mol) in THF (50 ml) at 0 C. under nitrogen atmosphere and then allowed to stir at room temperature for overnight. The reaction mixture was quenched with 6(N) KOH (5 ml) 0 C. and stirred with THF (50 ml) for another 30 minutes. The reaction mixture was filtered and the residue was washed with ethyl acetate. The filtrate was concentrated to give the crude amine. Satd. HCl in diethyl ether (20 ml) was added to the solution of crude amine in diethyl ether (20 ml) and stirred for 2 h. Then the reaction mixture was filtered and residue was dried to give the title compound (10 g, 97.08

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; ASTRAZENECA AB; US2008/15237; (2008); A1;,
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Application of 13726-21-1, 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. 13726-21-1, name is 2-(4-Chloro-3-methoxyphenyl)acetonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Gaseous HCl was slowly bubbled into a cooled solution of 4-chloro-3-methoxyacetonitrile (9b) in toluene (10 mL), ether (10 mL) and EtOH (1 mL) for about 10 min. The reaction was stoppered and stored at -30 C. for one week. TLC failed to detect any remaining starting material. The solvent was evaporated and the yellow solid was stirred with Et2O, filtered and washed with Et2O and dried in a vacuum oven to yield 0.57 g (90%) of ethyl 4-chloro-3-methoxyphenylmethylimidate (9d).

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-(4-Chloro-3-methoxyphenyl)acetonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Roche Palo Alto LLC; US2004/192704; (2004); A1;,
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Application of 447-60-9, 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 447-60-9 as follows.

Step B 7-Chloro-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one; [Show Image] A 1.8 M lithium diisopropylamide THF solution (45.3 ml, 81.6 mmol) was diluted with THF (68 ml). Thereafter, a solution obtained by dissolving the 5-chloro-2,N-dimethylbenzamide (5.0 g, 27.2 mmol) prepared in step A in THF (28 ml) was added dropwise to the diluted solution at -78C. Thereafter, a solution obtained by dissolving 2-trifluoromethylbenzonitrile (4.65 g, 27.2 mmol) in THF (28 ml) was further added thereto, and the obtained mixture was then stirred at -78C for 2.5 hours. The temperature of the reaction solution was increased to a room temperature, and a saturated ammonium chloride aqueous solution was added thereto, followed by extraction with ethyl acetate. The extract was washed with a saturated saline solution, and was then dried over anhydrous sodium sulfate. Thereafter, a solid generated as a result of vacuum concentration was filtrated, so as to obtain 7-chloro-3-(2-trifluoromethylphenyl)-2H-isoquinolin-1-one (6.87 g; yield: 78%) in the form of a colorless solid. 1H-NMR (270MHz, CDCl3) delta (ppm): 6.49 (1H, s), 7.33-7.72 (5H, m), 7.81-7.84 (1H, d, J=7.26Hz), 8.32-8.33 (1H, d, J=1.65Hz), 9.18 (1H, brs) ESI (LC-MS positive mode) m/z 324 (M+H).

According to the analysis of related databases, 447-60-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CHUGAI SEIYAKU KABUSHIKI KAISHA; EP1854792; (2007); A1;,
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These common heterocyclic compound, 38469-84-0, name is 5-Methoxy-2-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. name: 5-Methoxy-2-nitrobenzonitrile

General procedure: Condition B: An oven-dried pressure tube (10 mL) was charged with sodium sulfide nonahydrate (144 mg, 0.6 mmol), acetic acid (36 mg, 0.6 mmol), nitrobenzene (24.6 mg, 0.2 mmol), DMF (0.8 mL). The reaction vessel was closed under air and the resulting solution was stirred at room temperature for 20 h. Then the reaction mixture was filtered through a pad of silica gel and washed with 5 mL ethyl acetate for three times. The filtrate was removed under vacuum and the residue was purified by flash column chromatography (silica gel, petroleum ether/ethyl acetate = 4:1) to give the desired product.

The synthetic route of 5-Methoxy-2-nitrobenzonitrile has been constantly updated, and we look forward to future research findings.

Reference:
Article; Shuai, Qi; Li, Jun; Zhao, Feng; Su, Weike; Deng, Guojun; Chemical Papers; vol. 73; 4; (2019); p. 965 – 975;,
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Electric Literature of 886500-41-0,Some common heterocyclic compound, 886500-41-0, name is 4-Chloro-2,6-difluorobenzonitrile, molecular formula is C7H2ClF2N, 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.

A mixture of 4-chloro-2,6-difluorobenzonitrile (1.66 g, 9.56 mmol), pyrrole (0.67 g, 10 mmol) and Cs2CO3 (3.7 g, 12 mmol) in DMF (20 ml) was stirred overnight. Then, the solid was filtered off and the solvent was removed by reduced pressure. The residue was purified by column chromatography over silica gel (eluent: EtOAc/petroleum ether 10/1). The desired fractions were collected and the solvent was evaporated. Yield: 1.1 g of intermediate 15 (15% yield; white solid).

The synthetic route of 886500-41-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Meerpoel, Lieven; Maes, Louis Jules Roger Marie; de Wit, Kelly; US2013/85136; (2013); A1;,
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Synthetic Route of 20925-24-0, 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. 20925-24-0, name is 2-(Dimethylamino)benzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a stirred mixture of FeCl36H2O (270.3 mg, 1.0 mmol) and2.0 mL toluene was added aniline 1 (0.4 mmol) at room temperature.The reaction mixture was stirred at 85 C for 2 h in atmosphere.After it was cooled to room temperature, the reactionmixture was quenched by aqueous ammonia solution (mass fraction:25e28%, 10 mL) and extracted with dichloromethane (10 mLper time) until no product was observed in the extract, monitoredby TLC. The organic layer was dried over anhydrous MgSO4, filtered,and concentrated under reduced pressure to give crude product,which was chromatographed on silica gel column using 1:100 to1:70 (v/v) EtOAc/petroleum ether solutions as eluent to affordisolated product 2.

The synthetic route of 2-(Dimethylamino)benzonitrile has been constantly updated, and we look forward to future research findings.

Reference:
Article; Pan, Jing; Li, Jiaqiang; Huang, Ruofeng; Zhang, Xiaohui; Shen, Hang; Xiong, Yan; Zhu, Xiangming; Tetrahedron; vol. 71; 33; (2015); p. 5341 – 5346;,
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