HRID1975370

反应详情

EQUATION

反应方程式

HRID 1975370 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The starting material is prepared as follows: 3 g of isatic acid anhydride are dissolved in 50 ml of distilled hexametapol(=hexamethylphosphoric acid triamide). The solution is cooled to 5°, and 0.96 g of 55% NaH (freed of oil with hexane) is added. The mixture is stirred for 30 minutes at RT and then 5.67 g of O-(2-isopropyloxyethyl) tosylate are added. The mixture is stirred for 30 minutes at RT and for one hour at 50°. The mixture is left to stand overnight and is poured onto ice, and the organic layer is separated off and washed with water. The mixture is concentrated by evaporation, and the residue is digested with ether and filtered off with suction, yielding N-(2-isopropyloxyethyl)isatic acid anhydride, m.p. 107°-108°.

WORKUP

后处理

  1. customThe starting material is prepared
  2. temperatureThe solution is cooled to 5°
  3. stirringThe mixture is stirred for 30 minutes at RT and for one hour at 50°
  4. waitThe mixture is left
  5. waitto stand overnight
  6. additionis poured onto ice
  7. customthe organic layer is separated off
  8. washwashed with water
  9. concentrationThe mixture is concentrated by evaporation
  10. filtrationfiltered off with suction