HRID1803020

反应详情

EQUATION

反应方程式

HRID 1803020 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methanol (4 lt), 3-(3-chloropropoxy)-4-methoxy-6-nitro benzaldehyde (560 gm) and 30% methanolic NaOH solution (5 ml) were heated to 45° C. To this reaction mass 35% of H2O2 solution (1200 ml) was added drop wise in 3-4 hours maintaining a pH of 10.5-11.5 with 30% methanolic NaOH solution. The reaction mass was quenched into ice water (10 kg) and the pH adjusted to 2.0-3.0 using hydrochloric acid. The solid obtained was filtered, washed with 50% aqueous methanol (500 ml) and dried at 45-50° C. to yield the title compound (510 gm, 86% yield).

WORKUP

后处理

  1. customThe reaction mass was quenched into ice water (10 kg)
  2. customThe solid obtained
  3. filtrationwas filtered
  4. washwashed with 50% aqueous methanol (500 ml)
  5. customdried at 45-50° C.