HRID646075

反应详情

EQUATION

反应方程式

HRID 646075 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 6-methyl-1H-indole-3-carbaldehyde (0.96 g, Lit. 5) in methanol (15 ml) was added at 22° C. acetic acid (1.7 ml) and a solution of methylamine in tetrahydrofurane (2 M, 12.0 ml). After stirring for 1 h, sodium cyanoborohydride (0.76 g) was added in 5 portions and stirring was continued for 2 h. The mixture was evaporated and the residue partitioned between aqueous hydrochloric acid (1 N) and dichloromethane. The pH of the aqueous layer was adjusted to 14 using sodium hydroxide followed by extraction with dichloromethane. The organic layer was dried and evaporated to give crude methyl-(6-methyl-1H-indol-3-ylmethyl)-amine.

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued for 2 h
  3. customThe mixture was evaporated
  4. customthe residue partitioned between aqueous hydrochloric acid (1 N) and dichloromethane
  5. extractionfollowed by extraction with dichloromethane
  6. customThe organic layer was dried
  7. customevaporated