ChemicalBook CAS DataBase List 2-Chloronicotinamide

2-Chloronicotinamide synthesis

7synthesis methods

Product Name:2-Chloronicotinamide
CAS Number:10366-35-5
Molecular formula:C6H5ClN2O
Molecular Weight:156.57

6602-54-6

10366-35-5

General procedure for the synthesis of 2-chloronicotinamide from 2-chloro-3-cyanopyridine: 400 mL of concentrated sulfuric acid was added to a 1000 mL three-necked flask, followed by the addition of 2-chloro-3-cyanopyridine (138 g, 1 mol), which was stirred until completely dissolved. The reaction system was warmed up to 90 °C and the reaction was maintained at this temperature with stirring for 2 hours. Upon completion of the reaction, the reaction mixture was slowly poured into a mixture containing 1000 mL of ammonia and 1 kg of ice and stirring was continued for 1 hour. The precipitated crude product was collected by filtration. The crude product was transferred to 1000 mL of ethyl acetate and stirred for 1 hour to wash and subsequently separated by filtration to give a white solid product. Finally, the white solid was dried by blowing at 50 °C to give 153 g of the intermediate 2-chloronicotinamide as a white solid in 98% yield.

6602-54-6
510 suppliers
$6.00/10g

10366-35-5
203 suppliers
$9.00/10g

Yield:10366-35-5 98%

Reaction Conditions:

Stage #1:2-chloro-3-pyridinecarbonitrile with sulfuric acid at 90; for 2 h;
Stage #2: with ammonium hydroxide for 1 h;Cooling with ice;

Steps:

1 Preparation of 2-Chloronicotinamide (Compound B)
To 1000ml three-necked flask was added concentrated sulfuric acid 400ml, 2-chloronicotinonitrile (138g, 1mol), completely dissolved, warmingTo 90 ° C, stirred for 2 hours,The reaction mixture was poured into a mixture of 1000 ml of ammonia water and 1 kg of ice and stirred for 1 hour. After filtration, the crude solid was obtained by filtration. The crude product was added to 1000 ml of ethyl acetate, stirred for 1 hour and separated by filtration to obtain a white solid. The white solid was further dried by blowing at 50 ° C to afford 153 g of the intermediate 2-chloronicotinamide as a white solid in 98% yield.

References:

Beijing Ha Sanlian Science And Technology Co., Ltd.;Harbin Sanlian Pharmaceutical Co., Ltd.;Liu Jinai;Li Yuanzhen;Ning Ruibo;Wang Mingxin CN105367571, 2017, B Location in patent:Paragraph 0014; 0037; 0038

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