反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringunder violent stirring at 10° C
- stirringAfter stirring for 2 hours at 10° C.
- stirringAfter stirring for 2 hours
- filtrationthe mixture was filtered
- additionthe filtrate was mixed with 200 ml of chloroform
- washwashed twice with 200 ml of distilled water
- temperatureThe organic phase was cooled
- customto produce solid material, which
- filtrationwas recovered by filtration
- customThe solid material was dried
- customrecrystallized from acetone