HRID845828

反应详情

EQUATION

反应方程式

HRID 845828 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To 20 ml of methanol, 0.2 g of platinum oxide was added and then hydrogen was passed through the solution to activate the catalyst. To the solution was added a solution of 10.81 g (60 mmol) of 2-methoxy-3,4-methylenedioxybenzaldehyde (1) and 6.37 g (60 mmol) of aminoacetaldehyde dimethylacetal (99% purity) in 20 ml of ethanol to carry out hydrogenation for 3.5 hours. Then, 5.24 ml of 35% formaline (66 mmol) was added to carry out further hydrogenation for 9 hours. The catalyst was filtered out and the filtrate was concentrated under reduced pressure to obtain 16.85 g of N-(2-methoxy-3,4-methylenedioxybenzyl)-N-methylaminoacetaldehyde dimethylacetal (5) as an oil. Yield: 99%.

WORKUP

后处理

  1. customfor 3.5 hours
  2. customfor 9 hours
  3. filtrationThe catalyst was filtered out
  4. concentrationthe filtrate was concentrated under reduced pressure