HRID262990
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
- 30 °C
PROCEDURE
实验过程
1 g of 2-chloro-4-(o-chlorophenyl)-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine-9-methanol is dissolved in 10 ml of absolute pyridine and treated with 1 ml of acetic anhydride. The solution is maintained at 30° C. for 15 hours and then evaporated under vacuum. The residue is partitioned between methylene chloride and water. The organic phase is washed with saturated sodium chloride solution, dried over sodium sulphate and evaporated. By recrystallization of the residue from ethyl acetate, there is obtained 9-acetoxymethyl-2-chloro-4-(o-chlorophenyl)-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]-diazepine of melting point 191°-193° C.
WORKUP
后处理
- customevaporated under vacuum
- customThe residue is partitioned between methylene chloride and water
- washThe organic phase is washed with saturated sodium chloride solution
- dry with materialdried over sodium sulphate
- customevaporated
- customBy recrystallization of the residue from ethyl acetate