Category: nitriles-buliding-blocks

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. 35202-54-1, name is 4,5-Dimethoxy-1-cyanobenzocyclobutane, A new synthetic method of this compound is introduced below., SDS of cas: 35202-54-1

Example 1Charge 200 g of 3,4-dimethoxybicyclo [4.2.0]octa-l,3,5-triene-7-carbonitrile (I) in a 20.0 L 4- neck RB (round bottom) flask equipped with mechanical stirrer and thermometer pocket at 250C. Add 8 L of methanol, 40.2 g of nickel chloride hexahydrate and 461.5 g of boc anhydride (Di-tert-butyl dicarbonate) at 25°C. Cool the reaction mixture at -10 to 0°C and add 280.0 g of NaBH4 portion wise over 1 hour while maintaining the temperature of reaction mixture between -10 to 0°C. Remove the cooling bath, raise the temperature to 25°C and maintain for 2 hours. Monitor the reaction by HPLC and when the HPLC indicates the completion of the reaction (Compound (I) less than 0.2percent), charge 174.6 g of diethylene triamine at 250C. Stir for 1 hour at 25°C. Evaporate the methanol under vacuum to yield a black gummy residue. Charge 7 L of ethyl acetate in to the above residue. Charge 7 L of 10percent NaHCO3 solution. Stir for 15 minutes and separate the layers. Wash ethyl acetate layer with 7 L of water and dry the organic layer over anhydrous Na2SO4 and concentrate under vacuum at 50 – 55°C to obtain an off-white colored solid (II).Weight: 270. 0 g Yield: 87.0percent HPLC purity: 96.0percent

The synthetic route of 35202-54-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KRKA, D. D., NOVO MESTO; BOSE, Prosenjit; SIRIPALLI, Udaya Bhaskara Rao; KANDADAI, Appan Srinivas; WO2010/72409; (2010); A1;,
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1194-02-1, name is 4-Fluorobenzonitrile, 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. Product Details of 1194-02-1

A mixture of 4-fluorobenzonitrile (5 g, 41.3 mmol), dibutyltin oxide (2.055 g, 8.26 mmol), and trimethylsilyl azide (8.22 mL, 61.9 mmol) in toluene (165 mL) was heated to 100 C and stirred for 16.5 hours. After cooling to room temperature, the organic layer was extracted with NaOH 1 M (83 mL) and the aqueous layer was washed with EtOAc (2 x 85 mL). The aqueous layer was acidified with HCI 2M (41.3 mL) to pH 2. The aqueous mixture was extracted twice with EtOAc (200 mL then 100 mL) and the combined organic layers were washed with brine (60 mL), dried over anh. MgS04, filtered and concentrated to dryness to give Intermediate 1A, (5-(4- fluorophenyl)-2H-tetrazole, 6.61 g, 98% yield) as a white solid; H NMR (400 MHz, DMSO-d6) delta ppm 7.42 – 7.53 (m, 2 H) 8.04 – 8.14 (m, 2 H); MS m/z 165.2 (M+H)+; HPLC >99.5%, RT = 1.96 minutes.

The synthetic route of 1194-02-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UNIVERSITE DE MONTREAL; BC CANCER AGENCY; FRED HUTCHINSON CANCER RESEARCH CENTER; SAUVAGEAU, Guy; HUMPHRIES, Keith Richard; KIEM, Hans-Peter; FARES, Iman; CHAGRAOUI, Jalila; (122 pag.)WO2016/41080; (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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Application of 327-74-2, The chemical industry reduces the impact on the environment during synthesis 327-74-2, name is 2-Amino-5-cyanobenzotrifluoride, I believe this compound will play a more active role in future production and life.

General procedure: A solution of NaHCO3 (0.82 g) in distilledwater (4 mL) was stirred for 10 minutes and to it was added DCM (4 mL) followedby the different aniline 6-9, 11(2.4 mmol). The reaction mixture was cooled to 0 C, thiophosgene (0.3 mL, 3.7mmol) was added dropwise over 10 minutes and the reaction was then stirred atr.t. o.n. The mixture was then diluted with DCM (20 mL), washed with brine (20mL), the organic layer was dried over Na2SO4 andconcentrated to dryness.

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-Amino-5-cyanobenzotrifluoride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Ferla, Salvatore; Bassetto, Marcella; Pertusati, Fabrizio; Kandil, Sahar; Westwell, Andrew D.; Brancale, Andrea; McGuigan, Christopher; Bioorganic and Medicinal Chemistry Letters; vol. 26; 15; (2016); p. 3636 – 3640;,
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Reference of 613-46-7, A common heterocyclic compound, 613-46-7, name is 2-Naphthonitrile, molecular formula is C11H7N, 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: Benzonitrile 1a (1 mmol), Na2S*9H2O (1.2 mmol) and DMF (1 mL) were added into a 10 mL bottle. The reactor was placed in a heating magnetic stirrer at 130 C. After 2.5 h, by adding about 3 mL H2O after the reaction to disperse the solid product, the reaction mixture was extracted with EtOAc (3 x 3 mL), and the mixture was purified by column chromatography.

The synthetic route of 613-46-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Cao, Xian Ting; Yang, Huiyong; Zheng, Hui; Zhang, Pengfei; Heterocycles; vol. 96; 3; (2018); p. 509 – 517;,
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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. 610-66-2, name is 2-(2-Nitrophenyl)acetonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 2-(2-Nitrophenyl)acetonitrile

In a 1000ml three-necked round bottom flask equipped with a mechanical stirrer, thermometer and condenser, add 2-nitrophenylacetonitrile (32g, 0.2mol), 2-chloro-4,6-dimethoxy-1,3 5-Triazine (53 g, 0.3 mol), N, N-dimethylformamide (400 mL), stirred for 10 minutes, after the reaction material is dissolved, potassium carbonate (41 g, 0.3 mol) is added, and then the temperature is raised to 90 degrees to react 24 hours.After monitoring the reaction, the system was naturally cooled to room temperature, and the next oxidation operation was directly performed. Under mechanical agitation, 30% hydrogen peroxide (91 g, 0.8 mol) was slowly added dropwise to the system cooled down to room temperature to control the system temperature not to exceed 70 degrees.After the dropwise addition, the mixture was stirred at room temperature for 10 hours. Pour into 500mL of water and stir, the solid is precipitated and filtered directly,Wash the filter cake with a small amount of water to obtain 40 g of solid product (4,6-dimethoxy-1,3,5-triazin-2-yl) (2-nitrophenyl) methanoneThe yield is 70%.

The synthetic route of 610-66-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Anhui Chemical Institute; Luo Hongwen; Zhang Jiaxing; Xu Shouming; Mei Liyun; Fan Zhen; (11 pag.)CN110981825; (2020); A;,
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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. 6136-68-1, name is 3-Acetylbenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 3-Acetylbenzonitrile

i) Production of 3-(bromoacetyl)benzonitrile 3-Acetylbenzonitrile (5.33 g) and copper(II) bromide (16.40 g) were suspended in ethyl acetate (100 ml) and the mixture was heated under reflux for 2 hrs. After cooling the reaction mixture, the insoluble material was filtered off and the filtrate was washed with aqueous sodium hydrogen carbonate and saturated brine. The organic layer was dried and concentrated and the residue was recrystallized from ethyl acetate-diisopropyl ether to give the title compound (4.29 g) as colorless powder crystals. 1H-NMR (CDCl3)delta: 2.82 (2H, s), 6.06 (1H, t, J=7.8 Hz), 6.29 (1H, d, J=7.8 Hz), 6.57 – 6.72 (2H, m). IR (KBr): 3104, 2942, 2230, 1709, 1599 cm-1.

According to the analysis of related databases, 6136-68-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Takeda Chemical Industries, Ltd.; Kusaka, Masami; EP1348706; (2003); 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. 628-20-6, name is 4-Chlorobutyronitrile, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 628-20-6

A solution of 4-chlorobutyronitrile (2.5 mmol) in dimethylformamide (1 mL) was added during 1.5h to a mixture of the arylamine (2.5 mmol), Cs2CO3 (2.5 mmol) and KI (5 mmol) in dimethylformamide (4 mL). The mixture was stirred at the indicated temperature and time. After completion of the reaction, as indicated by TLC, the mixture was treated with ethyl ether (50 mL) and water (10 mL). The aqueous phase was separated and extracted with ethyl ether (30 mL). The combined organic layers were dried over anhydrous sodium sulphate and filtered. The solvent was evaporated in vacuo. The crude product was purified by column chromatography (Silica gel, hexane:DCM).

According to the analysis of related databases, 628-20-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Diaz, Jimena E.; Bisceglia, Juan A.; Mollo, Ma. Cruz; Orelli, Liliana R.; Tetrahedron Letters; vol. 52; 16; (2011); p. 1895 – 1897;,
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Adding a certain compound to certain chemical reactions, such as: 40497-11-8, name is Ethyl 2,3-dicyanopropanoate, 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 40497-11-8, COA of Formula: C7H8N2O2

Example 11 Preparation of 5-aminopyrazole (VII) [0071] To 2,6-dichloro-4-trifluoromethyl aniline 230 g and acetic acid 150 ml was added 1.1 m of nitrosyl sulphuric acid over one hour at 30 C. and maintained at 30 C. for one more hour. Heat the mass to 50-55 C. over ½ hour and the absence of 2,6-dichloro-4-trifluoromethyl aniline was monitored. Cool the mass to 30 C., and the excess nitrosyl sulphuric acid was destroyed. [0072] The above diazotized mass was added to a mixture of 250 ml of acetic acid, 162 g ethyl-2,3-dicyanoproprionate and 425 ml water over 4-5 hours maintaining temperature 0-5 C. Further maintained at 0 C./2 hours, 5 C./1 hour, 10 C./1 hour, 15 C./1 hour. 800 ml water was added at 15 C. over ½ hour, extracted the solution with 3×250 ml methylene dichloride. Layers were separated. Dichloromethane layer was washed with 250 ml water, cooled the dichloromethane layer to 0 C. and washed with 250 ml 8N aq. NH3 under stirring for one hour. Layers were separated, dichloromethane layer was taken and NH3 gas was passed at 0-5 C. till free NH3 was observed on top of the condenser and maintained the reaction mass for 3-4 hours at 0-5 C. Then 250 ml water was added, stirred for ½ hour, layers were separated, extracted aq. layer with 2×100 ml dichloromethane, dichloromethane layer was dried with MgS04, dichloromethane layer was concentrated to dryness, to obtain 288 g of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethyl phenyl)-pyrazole of 98% purity.

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, Ethyl 2,3-dicyanopropanoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Gharda, Keki Hormusji; US2013/30190; (2013); A1;,
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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 17823-40-4 as follows. Quality Control of 4-Bromo-2,3,5,6-tetrafluorobenzonitrile

A mixture of Compound G (6 50 g, 14.93 mmol), 4-bromo-2,3,5,6-tetrafluorobenzonitrile (3.86 g, 15.23 mmol), Pd(PPh3)4 (871 mg, 0.747 mmol), potassium carbonate (6 21 g, 44.79 mmol) in degassed deionized water (20 mL) and degassed THF (60 mL) solution was stirred at 80 C under a nitrogen atmosphere for 24 h. After cooled to room temperature, the reaction mixture was added methanol (400 mL) and filtered. The obtained solid was sequentially rinsed by water (20 mL) and methanol (20 mL), and eventually dried in vacuo. The obtained residue veas purified by column chromatography on silica gel using 3: 1 (v/v) hexane/toluene as eluent to afford a white solid (4 80 g, 66.6%). H NMR (500 MHz, CDCb, d): 8 94 (d, ./= 6.5 Hz, 2H), 8 80 (d, J= 7.0 Hz, 41 }. 7.70 (d, J= 8.5 Hz, 21 }. 7.66-7.59 (m, 6H); APCI-MS m/z: 483.4 ML

According to the analysis of related databases, 17823-40-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; KYULUX, INC.; CHENG, Shuo-Hsien; CHO, Yong, Joo; SUZUKI, Yoshitake; YANG, Yu, Seok; NOTSUKA, Naoto; ENDO, Ayataka; KAKIZOE, Hayato; YOSHIZAKI, Makoto; AGUILERA-IPARRAGUIRRE, Jorge; (264 pag.)WO2019/191665; (2019); A1;,
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