反应 #64971

反应方程式

sodium acetate

N-methylhydroxylamine hydrochloride

N-allyl-N-(2-oxopropyl)-acetamide

→

7-Acetyl-1,2-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane

溶剂

water

dioxane

反应条件

后处理

1. 1
   温度The mixture is heated
2. 2
   温度under reflux overnight
3. 3
   温度cooled
4. 4
   过滤the salts are filtered off with suction
5. 5
   洗涤washed with dioxane
6. 6
   浓缩The filtrate is concentrated
7. 7
   workup.ADDITIONK2CO3 is added
8. 8
   萃取The mixture is extracted with CHCl3
9. 9
   干燥the extract is dried over K2CO3
10. 10
    浓缩concentrated
11. 11
    workup.DISTILLATIONthe residue is distilled

实验过程

15.5 g (0.1 mol) of N-allyl-N-(2-oxopropyl)-acetamide are dissolved in 100 ml of dioxane, and 9 g of anhydrous sodium acetate and 9 g (0. 108 mol) of N-methylhydroxylamine hydrochloride in 10 ml of water are added. The mixture is heated under reflux overnight and cooled and the salts are filtered off with suction and washed with dioxane. The filtrate is concentrated, the residue is taken up in 100 ml of water and K2CO3 is added. The mixture is extracted with CHCl3, the extract is dried over K2CO3 and concentrated and the residue is distilled.

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