HRID2121287

反应详情

EQUATION

反应方程式

HRID 2121287 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

18.9 g of 1-benzyl-4-methylaminopiperidine as the oil prepared according to a) are taken up in 250 ml of methanol and combined with 8.3 g of cyclopropanecarboxaldehyde and 11.3 g of sodium cyanoborohydride. The mixture is stirred for 5 hours at 40-50° C., then for about another 16 hours at ambient temperature. It is then acidified with 2 N hydrochloric acid, evaporated to dryness in vacuo and the residue is taken up in water. It is washed with ether, made alkaline with concentrated sodium hydroxide solution and extracted with ether/ethyl acetate. The organic extract is dried over sodium sulphate and freed from the solvents in vacuo. 22.7 g 1-benzyl-4-(cyclopropylmethyl-methyl-amino)-piperidine are obtained as a yellowish oil.

WORKUP

后处理

  1. customfor about another 16 hours
  2. customat ambient temperature
  3. customevaporated to dryness in vacuo
  4. washIt is washed with ether
  5. extractionextracted with ether/ethyl acetate
  6. extractionThe organic extract
  7. dry with materialis dried over sodium sulphate