Tag: M.W=100-200

Some common heterocyclic compound, 25808-30-4, name is 2-(Methylamino)acetonitrile hydrochloride, molecular formula is C3H7ClN2, 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: 2-(Methylamino)acetonitrile hydrochloride

54.5 g of ethyl chloroformate was then poured dropwise into the resulting mix, with the temperature being maintained at between 0° and 5° to form a mixed anhydride. When the addition operation was concluded, agitation was effected for a further period of 30 minutes at 5° C. At the same time, 400 cc of chloroform and 55.5 g of triethylamine were introduced into a one liter balloon flask provided with an agitator and the mixture was cooled in an ice bath. 59 g of methylamino acetonitrile hydrochloride in finely divided form was then added gradually. The solution thus obtained was then gradually added to the solution of mixed anhydride which was produced previously, with the temperature being maintained at between 5° and 10°. At the end of the addition operation, agitation was effected for a further period of 1 hour at 5°C. The temperature of the reaction mix was permitted to rise and the reaction medium was left overnight. The chloroform was then distilled off under a slight vacuum. The residue was dissolved in water and the last traces of chloroform were removed by entrainment with water. The remaining product crystallized out. A few drops of soda lye were then added to make the medium slightly alkaline and then the product obtained was drained, washed with water until the Cl- ions were removed, and dried at 40°. Weight obtained=92 g MP=128° C. Yield=72.5percent

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 25808-30-4, its application will become more common.

Reference:
Patent; Societe d’Etudes Scientifiques et Industrielles de l’Ile-de-France; US4703055; (1987); A;,
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Synthetic Route of 34667-88-4, 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 34667-88-4 as follows.

Reference Example 114 4-Amino-2-fluorobenzonitrile To a solution of 2-fluoro-4-nitrobenzonitrile (2.51 g) in methanol (125 mL) was added 10% palladium carbon (50% 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, 70%). 1H-NMR (CDCl3)delta: 4.31 (2H, brs), 6.37-6.45 (2H, m), 7.31-7.36 (1H, m).

According to the analysis of related databases, 34667-88-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Takeda Pharmaceutical Company Limited; Kajino, Masahiro; Hasuoka, Atsushi; Tarui, Naoki; Takagi, Terufumi; EP2336107; (2015); B1;,
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Adding a certain compound to certain chemical reactions, such as: 117482-84-5, name is 3-Chloro-4-fluorobenzonitrile, 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 117482-84-5, Recommanded Product: 117482-84-5

A 1 L flask was charged with the product E obtained above (27.2 g 122.3 mmol, 1.0 equiv), 23.13 g 3-chloro-4-fluorobenzonitrile (122.3 mmol, 1.0 equiv), 49.8 g cesium carbonate (152.9 mmol, 1.25 equiv) and 200 mL DMF. The flask was equipped with a reflux condenser, and then placed into a preheated 110 C bath with stirring for 1 h under a dry N2 atmosphere. The resulting suspension was then cooled, diluted with H20 and extracted with 50% EtOAc/ Et20. The organics were washed with brine, dried with Na2S04 and concentrated under reduced pressure. Purification of the residue by flash chromatography (Si02, 20% EtOAc/Hexane) provided 33 g of the product as a white solid (90.4 mmol). ‘H NMR (500 MHz, CDC13): 8 1.86 (s, 3H), 2.82 (s, 1H), 6.80 (J= 8.5 Hz, 1H), 7.33 (dd, J = 8.5,1.5 Hz, 1 H), 7.59 (d, J= 8.5 Hz, 2H), 7.64 (s, 1H), 7.73 (d, J= 8.5 Hz, 2H).

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; AMGEN, INC.; WO2005/110980; (2005); A2;,
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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. 59997-51-2, name is 4,4-Dimethyl-3-oxopentanenitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 59997-51-2

At room temperature 4,4-dimethyl-3-oxopentanenitrile (J-ll) (1 equivalents, 5 g) was taken up in ethanol (100 mL), mixed with hydrazine hydrate (2 equivalents, 4.42 g) and refluxed for 3 h. The residue obtained after removal of the ethanol by distillation was taken up in water (100 mL) and extracted with ethyl acetate (300 mL). The combined organic phases were dried over sodium sulphate, the solvent was removed under vacuum and the product (J-lll) (5 g, 89 % yield) was obtained as a light red solid after recrystallisation from n- hexane (200 mL).

The synthetic route of 59997-51-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GRUeNENTHAL GMBH; FRANK, Robert; BAHRENBERG, Gregor; CHRISTOPH, Thomas; LESCH, Bernhard; WO2013/13815; (2013); 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. 628-20-6, name is 4-Chlorobutyronitrile, A new synthetic method of this compound is introduced below., HPLC of Formula: C4H6ClN

A mixture of l-methylimidazole (8.21g, 0.10 mmol) and Cl(CH₂)₃CN (12.43g, 0.12 mol)is stirred at 807deg;C for 24 hours. The resulting white solid is washed with diethyl ether (3 x 30 ml). The product is dried in vacuum for 24 hours. Yield: 17.6 g, 95%; M.p. 80C. ESI-MS(CH₃OH): Positive ion: 150 [C,sub>3CNmim], negative ion: 35 [Cl]. 1H NMR (CDCl₃): delta= 8.73 (s, 1H), 7.45 (s, 1H), 7.39 (s, 1H), 4.27 (t, J(H, H) = 6.8 Hz, 2H), 3.82 (s, 3H), 2.50 (t, J(H, H) = 6.8 Hz, 2H), 2.20 (t, J(H, H) = 6.8 Hz, 2H). ₁₃C NMR (CDCl₃): delta = 134.11, 130.49, 120.01, 116.19, 44.01,30.87, 21.21, 9.87. IR (cm-1): 3373, 3244, 3055 (V_C-H aromatic), 3029, 2974, 2949, 2927 (V_C-H aliphatic), 2243 (V_C-N), 1692 (V_C=N). Anal. Calcd for C₈H₁₂ClN₃ (%): C, 51.76, H, 6.51, N, 22.63; Found: C 51.72, H 6.55, N 22.71.

The synthetic route of 628-20-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ECOLE POLYTECHNIQUE FEDERALE DE LAUSANNE (EPFL); WO2005/19185; (2005); 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. 20925-24-0, name is 2-(Dimethylamino)benzonitrile, A new synthetic method of this compound is introduced below., Recommanded Product: 20925-24-0

To a solution of 2-dimethylamino-benzonitrile (300 mg, 2.1 mmol) in CH3OH (5 mL) and NET4OH (1 mL) was added Raney-Ni (100 mg). The reaction mixture was stirred at room temperature overnight under H2 balloon atmosphere. The suspension was filtered and the filter cake was washed with CH3OH (20 mL). The combined filtrate were concentrated to dryness to give the (2- aminomethyl-phenyl)-dimethyl-amine (200 mg, yield: quantitative) as colorless oil.

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; SANFORD BURNHAM PREBYS MEDICAL DISCOVERY INSTITUTE; GARDELL, Stephen; PINKERTON, Anthony B.; SERGIENKO, Eduard; SESSIONS, Hampton; (428 pag.)WO2018/132372; (2018); A1;,
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These common heterocyclic compound, 654-70-6, name is 4-Cyano-3-trifluoromethylaniline, 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. Recommanded Product: 654-70-6

To a solution of the acid chloride as prepared in the previous example (2.1 g, 0.0072 moles) in 12 mL of anhydrous toluene is added 0.9 g (0.0072 moles) of DMAP, maintaining the solution at room temperature; the suspension is allowed to react for 10 minutes then 1.15 g (0.0062 moles) of 4-amino-2-trifluoromethyl-benzonitrile dissolved in toluene is added and the mixture is heated at 75-80 C. (external temperature) for 8-10 hours following the disappearance of the amine by TLC (eluent: ethyl acetate/toluene 75/25 or CH2Cl2). After cooling to room temperature the solution is diluted with toluene and treated with a 5% solution of HCl, separated and washed with 5% bicarbonate solution. The organic phase is cured and evaporated under reduced pressure. Crude N-[4-cyano-3-(trifluoromethyl)-phenyl-]-3-[4-fluorophenylthio]-2-acetoxy-2-methyl-propionamide is obtained in quantitative yield as shown by HPLC analysis, NMR spectroscopy and TLC.

The synthetic route of 4-Cyano-3-trifluoromethylaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Pizzatti, Enrica; Vigano, Enrico; Lussana, Massimiliano; Landonio, Ernesto; US2006/41161; (2006); A1;,
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Related Products of 218632-01-0, The chemical industry reduces the impact on the environment during synthesis 218632-01-0, name is 3-Fluoro-4-nitrobenzonitrile, I believe this compound will play a more active role in future production and life.

The title compound was prepared following the procedure described in step-3, Intermediate80 by using 3-fluoro-4-nitrobenzonitrile (5 g, 30.i mmol), pyridin-3-ylmethanol (5.0 g, 45.i mmol), K2C03 (6.3 g, 45. i mmol) in DMF (30.0 mL) to afford 4.5 g of title compound:_To a solution of 4-iodo-3-(3-(pyridin-3-yloxy)propyl)benzoic acid (500 mg, i .30 mmol) inDMF (iO.0 mL) was added K2C03 (270 mg, i.95 mmol) and the reaction mass was stirred at60C for i h. Then added ethyl bromide (2i3 mg, i.95 mmol) and continued stirring at rt for4-5 h. The reaction mixture was quenched with water and filtered off precipitate to afford 500 mg of title compound.

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

Reference:
Patent; GLENMARK PHARMACEUTICALS S.A.; GHARAT, Laxmikant Atmaram; MUTHUKAMAN, Nagarajan; PISAL, Dnyandeo; KHAIRATKAR-JOSHI, Neelima; SHAH, Daisy Manish; KADAM, Sheetal R; (303 pag.)WO2016/55947; (2016); A1;,
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Some common heterocyclic compound, 1194-65-6, name is 2,6-Dichlorobenzonitrile, molecular formula is C7H3Cl2N, 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. Recommanded Product: 2,6-Dichlorobenzonitrile

EXAMPLE 37; N-{[1-(2-Cyclopropylethyl)-2-(2,6-dichlorophenyl)-4-hydroxy-6-oxo-1,6-dihydro-5-pyrimidinyl]carbonyl}glycine; 37a) 3-(2-Cyclopropylethyl)-2-(2,6-dichlorophenyl)-6-hydroxy-4(3H)-pyrimidinone; A 2 M solution of trimethylaluminium in hexane (1.38 mL, 2.76 mmol) was added to a stirred mixture of 2-(cyclopropyl)ethylamine hydrochloride (PCT Int. Appl. (2004), WO 2004052312, 0.305 g, 2.49 mmol), 2,6-dichlorobenzonitrile (0.516 g, 3.00 mmol) and toluene (5 mL) at room temperature. The mixture was stirred in a microwave reactor at 160 C. for 0.5 h, then cooled and the solvent removed under reduced pressure. Diethyl malonate (1.60 g, 10.0 mmol), 2-methoxyethanol (15 mL) and 4.37 M sodium methoxide in methanol (2.30 mL, 10.1 mmol) were added and the mixture refluxed under nitrogen for 18 h. After cooling, the mixture was poured into water (200 mL) containing 1 M aqueous sodium hydroxide (2 mL), washed with ether, acidified to pH 2 with 6 M aqueous hydrochloric acid, and extracted with ethyl acetate. The extracts were washed with water and brine, dried (MgSO4) and evaporated under reduced pressure. The residue was triturated with ether and the solid collected, washed with ether and dried to give the title compound (0.478 g, 59%) as a white solid. 1H NMR (400 MHz, DMSO-d6) delta ppm -0.29–0.20 (m, 2 H) 0.26-0.34 (m, 2 H) 0.44-0.60 (m, 1 H) 1.33-1.44 (m, 2 H) 3.60-3.72 (m, 2 H) 5.49 (s, 1 H) 7.66 (dd, J=9.09, 7.07 Hz, 1 H) 7.70-7.78 (m, 2 H) 11.80 (br. s., 1 H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1194-65-6, its application will become more common.

Reference:
Patent; Shaw, Antony N.; Duffy, Kevin J.; Tedesco, Rosanna; Wiggall, Kenneth; US2008/171756; (2008); A1;,
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Synthetic Route of 39581-21-0, 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. 39581-21-0, name is N-Butyl-2-cyano-acetamide belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A mixture of N-alkyl-2-cyano-acetamides 1a-c (2 mmol), aldehydes 2a-f (2 mmol),malononitrile (3) (2 mmol), K2CO3 (2 mmol), and EtOH (2 mL) in a 10 mL septum-capped microwavevials was irradiated under microwave conditions at 90 C, 500 W, 200 rpm, for 10-15 min. Aftercompletion of the reaction, as indicated by TLC, each vial was de-capped and the contents were left tocool to room temperature. Then, the reaction mixture was worked up as described in method I to givecompounds 4a-q. Analytical samples were obtained by recrystallization from MeOH.

The synthetic route of N-Butyl-2-cyano-acetamide has been constantly updated, and we look forward to future research findings.

Reference:
Article; Mekheimer, Ramadan Ahmed; Al-Sheikh, Mariam Abdullah; Medrasi, Hanadi Yousef; Alsofyani, Najla Hosain Hassan; Molecules; vol. 23; 3; (2018);,
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