HRID2293549

反应详情

EQUATION

反应方程式

HRID 2293549 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A 1.60 g portion of methyl 2,4-dimethoxy-5-formylaminobenzoate was dissolved in 20 ml of tetrahydrofuran, and 1.7 ml of borane dimethylsulfide complex was added under ice-cooling, followed by 2 hours of stirring at 60° C. Then, 3 ml of methanol and 4 ml of concentrated hydrochloric acid were added, followed by stirring at 75° C. for a while and then spontaneously cooled. The thus precipitated product of interest was collected by filtration, washed with tetrahydrofuran and then dried under a reduced pressure to give 1.08 g of methyl 2,4-dimethoxy-5-methylaminobenzoate.

WORKUP

后处理

  1. addition1.7 ml of borane dimethylsulfide complex was added under ice-
  2. temperaturecooling
  3. stirringby stirring at 75° C. for a while
  4. temperaturespontaneously cooled
  5. filtrationThe thus precipitated product of interest was collected by filtration
  6. washwashed with tetrahydrofuran
  7. customdried under a reduced pressure