HRID1600452
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
PROCEDURE
实验过程
To a solution of 8.0 g (0.045 mol) of 73 in 125 ml of toluene, 10 g (0.045 mol) of P4S10 was added. The suspension was refluxed for 4 h and left at room temperature overnight. The mixture was poured into ice water followed by basification with ammonia. The two-phase system was stirred with charcoal and filtered. The toluene phase was separated and the aqueous phase extracted with 2×100 ml of toluene. The combined organic phase were dried over MgSO4 and evaporated in vacuo leaving a heavy, yellow oil, 88. Yield: 2.3 g (0.013 mol), 29%).
WORKUP
后处理
- temperatureThe suspension was refluxed for 4 h
- filtrationfiltered
- customThe toluene phase was separated
- extractionthe aqueous phase extracted with 2×100 ml of toluene
- dry with materialThe combined organic phase were dried over MgSO4
- customevaporated in vacuo
- customleaving a heavy, yellow oil, 88