HRID1417967

反应详情

EQUATION

反应方程式

HRID 1417967 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

200 mg of 5-benzyloxy-4-methoxymethyl-9-{2-[N-methyl-N-(2-phenylethyl)-amino]-2-oxoethyl}-9H-pyrido[3,4-b]indole-3-carboxylic acid-(1-methylethyl)-ester is dissolved in 3 ml of tetrahydrofuran. Then, 0.29 ml of a 1.2 molar solution of diisobutylaluminum hydride in toluene is added in drops to the solution at 0° C., and it is stirred for 30 minutes at 0° C. Then, the reaction mixture is mixed with 0.1 ml of isopropanol and then with 0.1 ml of water, it is stirred for 2 hours at room temperature, filtered, and the filtrate is concentrated by evaporation in a vacuum. The residue is recrystallized from ethyl acetate, and 43 mg of 5-benzyloxy-4-methoxymethyl-9-{2-[N-methyl-N-(2-phenylethyl)-amino]-2-oxoethyl}-9H-pyrido[3,4-b]indole-3-carbaldehyde is obtained as colorless crystals with a melting point of 192°-197° C.

WORKUP

后处理

  1. filtrationfiltered
  2. concentrationthe filtrate is concentrated by evaporation in a vacuum
  3. customThe residue is recrystallized from ethyl acetate