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ChemicalBook CAS DataBase List 2-Chloronicotinamide

2-Chloronicotinamide synthesis

7synthesis methods
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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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