HRID645995
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 mixture of N-benzoyl-4-tert-butoxycarbonylaminomethyl-4-fluoropiperidine (step 3 of Example 15) (4.42 g, 13.1 mmol), NaOH (2.62 g, 65.5 mmol), H2O (9.00 mL) and ethanol (90.0 mL) was refluxed for 15 h and concentrated in vacuo. To the resulting residue were added water and chloroform. The organic layer was separated, dried over magnesium sulfate, and concentrated under reduced pressure. Recrystallization of the resulting solid with hexane-CH2Cl2 afforded a colorless solid 1.77 g (58%) as the titled compound.
WORKUP
后处理
- temperaturewas refluxed for 15 h
- concentrationconcentrated in vacuo
- additionTo the resulting residue were added water and chloroform
- customThe organic layer was separated
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customRecrystallization of the resulting solid with hexane-CH2Cl2