HRID1107607

反应详情

EQUATION

反应方程式

HRID 1107607 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into other 500 ml rounded-flask, were introduced 4.0 g of magnesium oxide and 80 g of distilled water. The mixture was stirred. Thereto was added 7.3 g of N,N'-bis(2-hydroxyethyl)-1,2-diaminoethane prepared above and 250 ml of 1,4-dioxane. 27.5 g of palmitoyl chloride was gradually added dropwise to the resulting mixture for 1 hour under violent stirring at a room temperature. After stirring for 2 hours, the mixture was filtered, and then the filtrate was mixed with 200 ml of chloroform and washed twice with 200 ml of distilled water. Organic phase was cooled to produce solid material, which was recovered by filtration. The solid material was dried and recrystallized from chloroform/acetone and chloroform/hexane, to give 24.3 g of the title compound as white powder, which was identified by IR and NMR. The results are shown in Table 3.

WORKUP

后处理

  1. stirringunder violent stirring at a room temperature
  2. stirringAfter stirring for 2 hours
  3. filtrationthe mixture was filtered
  4. additionthe filtrate was mixed with 200 ml of chloroform
  5. washwashed twice with 200 ml of distilled water
  6. temperatureOrganic phase was cooled
  7. customto produce solid material, which
  8. filtrationwas recovered by filtration
  9. customThe solid material was dried
  10. customrecrystallized from chloroform/acetone and chloroform/hexane