HRID2070874

反应详情

EQUATION

反应方程式

HRID 2070874 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

2-(2,4-Dimethoxybenzyl)-5-nitroisoindolin-1-one. A mixture of methyl 2-(bromomethyl)-4-nitrobenzoate (2.5 g, 9.12 mmol), (2,4-dimethoxyphenyl)methanamine (1.525 g, 9.12 mmol), triethylamine (3.81 mL, 27.4 mmol) in methanol (25 mL) was refluxed for 16 h. The mixture was diluted with ethyl acetate, washed with dilute hydrochloric acid and brine, dried over magnesium sulfate, filtered, and concentrated on a rotary evaporator to dryness. Flash chromatography (30-50% ethyl acetate in hexane) gave the desired product as a yellow solid (2.5 g, 7.68 mmol, 84% yield). MS (ESI) m/z 329.9 [M+1]+.

WORKUP

后处理

  1. temperaturewas refluxed for 16 h
  2. washwashed with dilute hydrochloric acid and brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated on a rotary evaporator to dryness