HRID1115

反应详情

EQUATION

反应方程式

HRID 1115 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

A 500-ml flask equipped with a stirrer and reflux condenser was charged with 3.01 g (79.3 mmol) of LiAlH4 and 200 ml of tetrahydrofuran. While stirring the mixture at room temperature in an N2 atmosphere, 5.00 g (13.9 mmol) of N,N-bis(2-hydroxyethyl)-16-hydroxyhexadecanamide were added, followed by stirring at 65° C. for 18 hours. After cooling the reaction mixture to room temperature, 15 g of 3% aqueous KOH were added, and a salt deposited was separated by filtration. The solvent was then distilled off under reduced pressure, and the resultant residue was purified by column chromatography on silica gel, thereby obtaining 2.98 g (yield: 62%) of the title compound (IId-3).

WORKUP

后处理

  1. customA 500-ml flask equipped with a stirrer
  2. temperaturereflux condenser
  3. additionwere added
  4. temperatureAfter cooling the reaction mixture to room temperature
  5. customa salt deposited was separated by filtration
  6. distillationThe solvent was then distilled off under reduced pressure
  7. customthe resultant residue was purified by column chromatography on silica gel