HRID1701107

反应详情

EQUATION

反应方程式

HRID 1701107 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

20 g of 2,6-diethyl-2,3,6-trimethyl-4-benzamidopiperidine (compound no. 9), 12.5 g of benzylbromide, 1 g of potassium iodide and 20 g of potassium carbonate are stirred in 200 ml of tetrahydrothiophene dioxide (sulpholane) at 110° C. for 4 days. Thereafter the reaction mixture is diluted with 200 ml of toluene, cooled to room temperature and purified by filtration. The filtrate is washed four times with about 200 ml of water, the toluene phase is dried over sodium sulfate and evaporated under vacuum. Crystallization of the residue from acetic acid ethyl ester yields 1-benzyl-2,6-diethyl-2,3,6-trimethyl-4-benzamidopiperidine (compound no. 48); m.p. 234°-236° C.

WORKUP

后处理

  1. filtrationpurified by filtration
  2. washThe filtrate is washed four times with about 200 ml of water
  3. dry with materialthe toluene phase is dried over sodium sulfate
  4. customevaporated under vacuum
  5. customCrystallization of the residue from acetic acid ethyl ester