HRID1282000
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 stirred mixture of 22.2 g (193 mmol) of 4-hydroxymethylpiperidine (Example 8) in 100 mL of CH2Cl2 and 75 mL of a 15% aqueous solution of NaOH was added a solution of 63 g (289 mmol) of Boc2O in 50 ml of CH2Cl2 over a period of 2 h. After stirring for 30 min, the organic layer of the reaction mixture was washed with 15% aqueous NaOH solution and sat'd NaCl solution, dried over MgSO4, filtered and the filtrate was concentrated. The residue was purified by chromatography (silica, hexanes:ethyl acetate=19:1, then 4:1) to give the title compound.
WORKUP
后处理
- washthe organic layer of the reaction mixture was washed with 15% aqueous NaOH solution
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationthe filtrate was concentrated
- customThe residue was purified by chromatography (silica, hexanes