HRID1282000

反应详情

EQUATION

反应方程式

HRID 1282000 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. washthe organic layer of the reaction mixture was washed with 15% aqueous NaOH solution
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationthe filtrate was concentrated
  5. customThe residue was purified by chromatography (silica, hexanes