HRID1155917
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureis heated at 100°-105° C. for 18 hours under nitrogen
- temperatureThe reaction mixture is cooled
- filtrationThe precipitate is filtered off
- washwashed with water, with acetone
- customdried
- customRecrystallization from dimethylformamide
- customgives a crystalline product (0.39 g.) mp 300° C. (dec)