HRID606700

反应详情

EQUATION

反应方程式

HRID 606700 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Anthranilonitrile (10.0 grams, 85.0 mmol) was dissolved in 350 mL of acetic acid. To this was added 2,5-dimethoxytetrahydrofuran (11.0 mL, 85.0 mmol). This was stirred at reflux for 2 hours after which time the reaction mixture was pored into water and the product extracted with dichloromethane. The organic layer washed with water, dried over sodium sulfate and chromatographed on a silica gel column using a mobile phase of 1:1 dichloromethane-hexane to afford the title compound as a white solid. NMR confirms structure.

WORKUP

后处理

  1. temperatureat reflux for 2 hours after which time the reaction mixture
  2. extractionthe product extracted with dichloromethane
  3. washThe organic layer washed with water
  4. dry with materialdried over sodium sulfate
  5. customchromatographed on a silica gel column