HRID846965

反应详情

EQUATION

反应方程式

HRID 846965 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 3.368 g (10.22 mM) of 3-hexadecyloxy-2-methoxypropylamine IV a3 in 35 ml of dichloromethane and 1.85 ml (13.29 mM) of triethylamine is added 1.99 g (11.24 mM) of 3-chloropropanesulfonyl chloride with ice-cooling and the mixture is stirred at room temperature for 4 hours and then heated for 30 minutes with stirring. After the solvent is evaporated, the residue is purified by the column chromatography on silica gel with a n-hexane-ethyl acetate (3:1) mixture as an eluent. The product is recrystallized form methanol to give 4.15 g (8.827 mM) of 3-(3-chloropropylsulfonylamino)-1-hexadecyloxy-2-methoxypropane III a3 as a colorless powder in 86% yield.

WORKUP

后处理

  1. temperaturecooling
  2. temperatureheated for 30 minutes
  3. stirringwith stirring
  4. customAfter the solvent is evaporated
  5. customthe residue is purified by the column chromatography on silica gel with a n-hexane-ethyl acetate (3:1) mixture as an eluent
  6. customThe product is recrystallized form methanol