HRID1107609

反应详情

EQUATION

反应方程式

HRID 1107609 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into a 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 in Example 27, and then was added 250 ml of 1,4-dioxane. 13.4 g of palmitoyl chloride was gradually added dropwise to the resulting mixture for 1 hour under violent stirring at 10° C. After stirring for 2 hours at 10° C., 14.7 g of oleoyl chloride was gradually added dropwise thereto for 1 hour. 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. The organic phase was cooled to produce solid material, which was recovered by filtration. The solid material was dried and recrystallized from acetone, to give 26.5 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 10° C
  2. stirringAfter stirring for 2 hours at 10° C.
  3. stirringAfter stirring for 2 hours
  4. filtrationthe mixture was filtered
  5. additionthe filtrate was mixed with 200 ml of chloroform
  6. washwashed twice with 200 ml of distilled water
  7. temperatureThe organic phase was cooled
  8. customto produce solid material, which
  9. filtrationwas recovered by filtration
  10. customThe solid material was dried
  11. customrecrystallized from acetone