Реакция #64975

Уравнение реакции

sodium acetate

N-methylhydroxylamine hydrochloride

ethyl N-(but-2-enyl)-N-(2-oxoethyl)-carbamate

→

Ethyl 2,4-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

Растворители

water

dioxane

Условия реакции

Обработка

1. 1
   ТемператураThe mixture is heated
2. 2
   Температураunder reflux overnight
3. 3
   Температураcooled
4. 4
   Фильтрацияthe salts are filtered off with suction
5. 5
   Промывкаwashed with dioxane
6. 6
   КонцентрированиеThe filtrate is concentrated
7. 7
   workup.ADDITIONK2CO3 is added
8. 8
   ЭкстракцияThe mixture is extracted with CHCl3
9. 9
   Сушкаthe extract is dried over K2CO3
10. 10
    Концентрированиеconcentrated
11. 11
    workup.DISTILLATIONthe residue is distilled

Методика

18.4 g (0.1 mol) of ethyl N-(but-2-enyl)-N-(2-oxoethyl)-carbamate 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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