HRID1598366
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 crude 4-benzyl-2-phthalimidomethylmorpholine (64 g) in ethanol (500 ml) was added hydrazine monohydrate (18 ml, 0.57 mol) and the mixture was heated under reflux for 2 hours. After cooling, 10% aqueous sodium hydroxide (200 ml) was added to dissolve insolubles and the ethanol was distilled off under reduced pressure. The aqueous layer was extracted with chloroform (200 ml×3), the combined organic layer was dried over potassium carbonate and the solvent was distilled off to give crude 2-aminomethyl-4-benzylmorpholine (42.97 g). This compound was used for the subsequent reaction without purification.
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 2 hours
- temperatureAfter cooling
- dissolutionto dissolve insolubles
- distillationthe ethanol was distilled off under reduced pressure
- extractionThe aqueous layer was extracted with chloroform (200 ml×3)
- dry with materialthe combined organic layer was dried over potassium carbonate
- distillationthe solvent was distilled off