HRID2245403

反应详情

EQUATION

反应方程式

HRID 2245403 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 4-[2-({[(1,1-dimethylethyl)oxy]carbonyl}amino)ethyl]-3-thiomorpholinecarboxylate 1,1-dioxide (D17; 295 mg, 0.88 mmol) in 3 ml of anhydrous dichloromethane was added 1 ml of trifluoroacetic acid and the resulting solution was stirred at room temperature under nitrogen for 1 h 30min. The solvent was removed under reduced pressure and the residue loaded on a SCX column, washed with methanol and eluted with methanolic ammonia. The product was purified further by chromatography (silica cartridge, cyclohexane to ethyl acetate, then dichloromethane to dichloromethane: methanol 70:30) to give 165 mg of the target compound.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. washwashed with methanol
  3. washeluted with methanolic ammonia
  4. customThe product was purified further by chromatography (silica cartridge, cyclohexane to ethyl acetate