HRID77760

反应详情

EQUATION

反应方程式

HRID 77760 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-Amino-1-(1,1-dioxo-1lambda*6*-thiomorpholin-4-yl)-propan-1-one (6.0 g, 18.2 mmol) and BH3 (1 M in THF, 110 mL) was heated to reflux for 48 h, then cooled to room temperature and quenched by MeOH. The volatile was removed under vacuum. 2 N HCl (100 mL) was added to the residue and heated to reflux for 18 h. Solvent was removed under vacuum to give (S)-2-(1,1-Dioxo-1lambda*6*-thiomorpholin-4-yl)-1-methyl-ethylamine (4.5 g) as white solid, yield 90%. MS (M+H)=193.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 48 h
  3. customquenched by MeOH
  4. customThe volatile was removed under vacuum
  5. addition2 N HCl (100 mL) was added to the residue
  6. temperatureheated
  7. temperatureto reflux for 18 h
  8. customSolvent was removed under vacuum