HRID2238487
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
Methyl 1-ethyl-5-oxo-prolinate (1.91 g, 11.17 mmol) was dissolved in methanol (25 ml) and treated with 2M aqueous sodium hydroxide (7.3 ml, 14.52 mmol). The mixture was stirred for 4 hrs at room temperature and then washed with dichloromethane. The aqueous layer was evaporated and the residue treated with an excess of 1M hydrogen chloride in ether (˜5 ml). The mixture was evaporated once more and the residue was triturated with dichloromethane. The solid material was discarded and the combined dichloromethane fractions were evaporated to give a clear oil which crystallized on standing. Trituration with hexane and ether and drying gave pure 1-ethyl-5-oxo-proline (0.271 g) as a white solid.
WORKUP
后处理
- washwashed with dichloromethane
- customThe aqueous layer was evaporated
- additionthe residue treated with an excess of 1M hydrogen chloride in ether (˜5 ml)
- customThe mixture was evaporated once more
- customthe residue was triturated with dichloromethane
- customthe combined dichloromethane fractions were evaporated
- customto give a clear oil which
- customcrystallized
- dry with materialTrituration with hexane and ether and drying