HRID2380681

反应详情

EQUATION

反应方程式

HRID 2380681 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2.76 g of N-(2'-cyanobiphenyl-4-ylmethyl)-N-propyl-isophthalic acid monoamide and 8.68 g of tributyltin azide in 75 ml of xylene is heated under reflux for 2 hours. When cool, the mixture is stirred with 50 ml of 2N sodium hydroxide solution at room temperature for 1 hour, and is then acidified and extracted with 100 ml and twice with 50 ml of CH2Cl2. After customary treatment, the combined dichloromethane phases yield a crude product that, after chromatography on silica gel 60 (40-63 μm) using CH2Cl2 /CH3OH (9:1) as eluant, yields N-propyl-N-[2'-(1H-tetrazol-5-yl)-biphenyl-4-ylmethyl]-isophthalic acid monoamide that has an Rf value of 0.10 [CH2Cl2 /CH3OH (4:1)]. ##STR10##

WORKUP

后处理

  1. temperatureunder reflux for 2 hours
  2. temperatureWhen cool
  3. extractionextracted with 100 ml and twice with 50 ml of CH2Cl2
  4. customAfter customary treatment, the combined dichloromethane phases yield a crude product that