HRID1063308

反应详情

EQUATION

反应方程式

HRID 1063308 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-Benzyl-3,3-dimethyl-4-piperidone 275 g (1.26 mol) prepared as per procedure described in U.S. Pat. No. 5,846,980, was dissolved in 1.0 L. methanol. The solution was transferred to a Parr reactor after adding 10% palladium on carbon (25 g). The reaction mixture was stirred under 300 psi hydrogen pressure at 60° C. until chromatography showed complete conversion. The reaction mixture was filtered and the residue washed with methanol (200 ml). The filtrate was concentrated to dryness to afford 3,3-dimethyl-4-piperidone (158 g) which was used as such for the preparation of either 4-benzyloxycarbonylamino-3,3-dimethylpiperidine or 4-t-butyloxycarbonylamino-3,3-dimethylpiperidine.

WORKUP

后处理

  1. dissolution5,846,980, was dissolved in 1.0 L
  2. filtrationThe reaction mixture was filtered
  3. washthe residue washed with methanol (200 ml)
  4. concentrationThe filtrate was concentrated to dryness