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
A solution of (RS)-5-[3-(benzhydrylidene-amino)-phenyl]-5-methyl-morpholin-3-one (5.62 g, 15 mmol) in dioxane (75 ml) was cooled to 15° C. and treated dropwise with 1 N hydrochloric acid (18 ml). The reaction mixture was stirred at room temperature overnight. For the workup, the reaction mixture was evaporated at reduced pressure, and the residue was portioned between diethylether (120 ml) and 1 N hydrochloric acid (20 ml). The aqueous phase was separated and washed with diethylether (120 ml). This procedure was repeated twice. The combined aqueous layers were evaporated at reduced pressure, and 3.27 g (88% of theory) of (RS)-5-(3-amino-phenyl)-5-methyl-morpholin-3-one hydrochloride were obtained as a yellowish solid used in the next step without further purification. Mass (calculated) C11H15ClN2O2 [242.707]; (found) [M+H]+=207.
WORKUP
后处理
- customFor the workup, the reaction mixture was evaporated at reduced pressure
- customThe aqueous phase was separated
- washwashed with diethylether (120 ml)
- customThe combined aqueous layers were evaporated at reduced pressure