HRID724781
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
- 150 °C
PROCEDURE
实验过程
A mixture of alpha-hydroxy-gamma-butyrolactone (22.0 g) and 3-trifluoromethoxy aniline (19.0 g) was heated to 150° C. (bath temperature) for 48 hours. The mixture was allowed to cool and poured into a mixture of diethyl ether and water. After shaking, the ether layer was separated and the aqueous layer extracted with diethyl ether (x2). The combined ether extracts were washed with 2M hydrochloric acid, water and brine, then dried (MgSO4). The mixture was evaporated under reduced pressure to leave an oil, which on trituration with a mixture of diethyl ether/hexane gave the sub-title compound as an off-white solid (19.42 g).
WORKUP
后处理
- temperatureto cool
- customthe ether layer was separated
- extractionthe aqueous layer extracted with diethyl ether (x2)
- washThe combined ether extracts were washed with 2M hydrochloric acid, water and brine
- dry with materialdried (MgSO4)
- customThe mixture was evaporated under reduced pressure
- customto leave an oil, which on trituration