HRID1061055

反应详情

EQUATION

反应方程式

HRID 1061055 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In dichloromethane (60 ml), 4-tert-butoxycarbonyl-1-[(3-hydroxy-1-propyl)sulfonyl]piperazine (3.00 g) was dissolved. To the resulting solution, diisopropylethylamine (2.72 ml) was added, followed by the addition of methoxymethyl chloride (1.11 ml) under ice cooling. After stirring at room temperature for 20 hours, the reaction mixture was diluted with dichloromethane, washed with water, a 5% aqueous citric acid solution and saturated saline and then dried over anhydrous sodium sulfate. The solvent was then distilled off under reduced pressure. The residue was purified by chromatography on a silica gel column (hexane:ethyl acetate=2:1), whereby the title compound (3.32 g, 97%) was obtained.

WORKUP

后处理

  1. washwashed with water
  2. dry with materiala 5% aqueous citric acid solution and saturated saline and then dried over anhydrous sodium sulfate
  3. distillationThe solvent was then distilled off under reduced pressure
  4. customThe residue was purified by chromatography on a silica gel column (hexane:ethyl acetate=2:1), whereby the title compound (3.32 g, 97%)
  5. customwas obtained