HRID1413212
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A solution of 4-acetylaminothiazole (2.85 g, 20 mM) in a mixture of acetic anhydride (30 ml) and pyridine (10 ml) was heated at 100° C. for 16 hours. The reaction mixture was cooled and poured onto an ice cold mixture of 20% aqueous sodium acetate (200 ml) and chloroform (200 ml.). The layers were separated the organic layer was washed with water, dried (MgSO4) and the solvents removed under vacuum to give an oil. Trituration with hexane followed by recrystallisation from di-isopropyl ether gave the title compound (1.8 g, 49%) m.p. 55° C. (Found: C, 45.8; H, 4.4; N, 15.5%. C7H8N2O2S requires: C, 45.6; H, 4.4; N, 15.2%)
WORKUP
后处理
- temperatureThe reaction mixture was cooled
- customThe layers were separated the organic layer
- washwas washed with water
- dry with materialdried (MgSO4)
- customthe solvents removed under vacuum
- customto give an oil
- customTrituration with hexane followed by recrystallisation from di-isopropyl ether