反応 #64971

反応方程式

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

溶媒

water

dioxane

反応条件

後処理

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

実験手順

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.

出典