HRID975080

反应详情

EQUATION

反应方程式

HRID 975080 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

The 3-(2-tetrahydropyranyloxyethyl)-3-(3,4-dichlorophenyl)-2-pyrrolidinone (3.9 grams prepared as described supra) is dissolved in 50 ml of tetrahydrofuran and the solution is added to a suspension of 0.9 grams of lithium aluminum hydride in 5 ml of tetrahydrofuran heated to 60° C. The reaction mixture is then heated for one hour at 60° C. and then cooled. To the resulting mixture 1 ml of water, 1 ml of 4N sodium hydroxide, and 3 ml of water are added sequentially. The insoluble portion is removed by filtration and the filtrate is concentrated in vacuo. The residue is taken up in diethyl ether, dried over magnesium sulfate, and concentrated under vacuum to give the desired intermediate.

WORKUP

后处理

  1. temperatureThe reaction mixture is then heated for one hour at 60° C.
  2. temperaturecooled
  3. customThe insoluble portion is removed by filtration
  4. concentrationthe filtrate is concentrated in vacuo
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under vacuum