HRID2236093

反应详情

EQUATION

反应方程式

HRID 2236093 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl (2-tert.-butoxycarbonyl-1,2,3,4-tetrahydro-pyrido[4,3-b]indol-5-yl)-acetate (8.45 g, 23.6 mmol) in ethyl acetate (80 ml) is treated with a solution of 3M HCl in ethyl acetate (39.3 ml). After stirring at room temperature for 3 h, the solvent is removed in vacuo and the residue azeotroped twice with toluene. The crude product is suspended in diethyl ether, filtered off, washed with diethyl ether and dried. Finally, pure title compound is obtained as beige solid (5.49 g) in 79% yield. tR (LC-2) 1.41 min; ESL-MS (positive ion): m/z 259.33 [M+H]+ (calcd 258.32 for C15H18N2O2).

WORKUP

后处理

  1. customthe solvent is removed in vacuo
  2. customthe residue azeotroped twice with toluene
  3. filtrationfiltered off
  4. washwashed with diethyl ether
  5. customdried