Реакция #64963

Уравнение реакции

water

N-methylhydroxylamine hydrochloride

sodium methylate

N-allyl-N-(1-oxoprop-2-yl)-urethane

→

methylhydroxylamine

Ethyl 2,8-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

Растворители

methanol

toluene

toluene

Условия реакции

Обработка

1. 1
   Другоеthe solution formed
2. 2
   Температураis heated
3. 3
   Температураunder reflux
4. 4
   ТемператураThe mixture is heated
5. 5
   Температураunder reflux overnight
6. 6
   Экстракцияthe product is extracted with dilute hydrochloric acid
7. 7
   Экстракцияextracted with CHCl3
8. 8
   СушкаThe extract is dried over K2CO3
9. 9
   Концентрированиеconcentrated
10. 10
    workup.DISTILLATIONthe residue is distilled

Методика

A methanolic methylhydroxylamine solution is prepared from 16.4 g (0.2 mol) of N-methylhydroxylamine hydrochloride in 33 ml of absolute methanol and 36 g (0.2 mol) of 30% strength sodium methylate solution, and the solution formed is diluted with 130 ml of toluene and added dropwise to 354 g (0.17 mol) of N-allyl-N-(1-oxoprop-2-yl)-urethane in 250 ml of toluene, which is heated under reflux using a water separator. The mixture is heated under reflux overnight, the product is extracted with dilute hydrochloric acid and the hydrochloric acid solution is rendered alkaline with K2CO3 and extracted with CHCl3. The extract is dried over K2CO3 and concentrated and the residue is distilled.

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