HRID1577422

反应详情

EQUATION

反应方程式

HRID 1577422 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 10-oxo-10H-pyrido[1,2-a]thieno[3,2-d]pyrimidine-7-carbonitrile (0.6 g., 0.0026 mol), sodium azide (0.56 g., 0.0086 mol) and ammonium chloride (0.46 g., 0.0036 mol) in dimethylformamide (75 ml) is heated at 100°-105° C. for 18 hours under nitrogen. The reaction mixture is cooled, poured into ice water (700 ml) and acidified with concentrated hydrochloric acid (1 ml). The precipitate is filtered off, washed with water, with acetone and dried. Recrystallization from dimethylformamide gives a crystalline product (0.39 g.) mp 300° C. (dec).

WORKUP

后处理

  1. temperatureis heated at 100°-105° C. for 18 hours under nitrogen
  2. temperatureThe reaction mixture is cooled
  3. filtrationThe precipitate is filtered off
  4. washwashed with water, with acetone
  5. customdried
  6. customRecrystallization from dimethylformamide
  7. customgives a crystalline product (0.39 g.) mp 300° C. (dec)