HRID1055331

反应详情

EQUATION

反应方程式

HRID 1055331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of formic acid (106 mL) and acetic anhydride (53.0 mL) was stirred at room temperature for 1 h. Methyl 3-aminobenzoate (8.50 g, 56.2 mmol) was added and the resulting mixture was stirred overnight. The reaction mixture was then concentrated under reduced pressure to give a solid. The solid was dissolved in THF (50.0 mL) and this solution was cooled to 0° C. Borane dimethylsulfide (10.7 mL, 112 mmol) was added slowly and the resulting mixture was stirred at room temperature overnight. The reaction mixture was then cooled to 0° C. and MeOH (10 mL) was added slowly. This mixture was stirred for 3 hours and then concentrated under reduced pressure to give the title compound, which was used without any further purification.

WORKUP

后处理

  1. concentrationThe reaction mixture was then concentrated under reduced pressure
  2. customto give a solid
  3. stirringthe resulting mixture was stirred at room temperature overnight
  4. temperatureThe reaction mixture was then cooled to 0° C.
  5. stirringThis mixture was stirred for 3 hours
  6. concentrationconcentrated under reduced pressure