HRID622192

反应详情

EQUATION

反应方程式

HRID 622192 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7.81 g (40 mmol) of 2-methoxy-3,4-methylenedioxybenzaldoxime (2) thus obtained, 3.67 ml (44 mmol) of concentrated hydrochloric acid and 500 mg of 5% palladium on carbon catalyst were added to 80 ml of ethanol to carry out hydrogenation at room temperature for 4 hours and 45 minutes. The catalyst was filtered out, the filtrate was concentrated and the residue is recrystallized from 60 ml of ethanol to obtain 4.86 g of 2-methoxy-3,4-methylenedioxybenzylamine hydrochloride (3). Yield 56%, m.p. 208°-210° C. IR and NMR spectra of the resultant product are listed below. ##STR29##

WORKUP

后处理

  1. customat room temperature
  2. customfor 4 hours
  3. custom45 minutes
  4. filtrationThe catalyst was filtered out
  5. concentrationthe filtrate was concentrated
  6. customthe residue is recrystallized from 60 ml of ethanol