반응 #216751

반응 방정식

5,8-dimethyl-6-bromothiochroman-4-one

O-methylhydroxylamine hydrochloride

ethanol

→

4-methoxyimino-5,8-dimethyl-6-bromothiochroman

수율 94.4%

용매

pyridine

반응 조건

후처리

1. 1
   온도under heat for 30 minutes
2. 2
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
3. 3
   workup.ADDITION50 ml of 5% hydrochloric acid was added
4. 4
   기타to form a solid
5. 5
   여과The solid was recovered by filtration
6. 6
   세척washed with water
7. 7
   기타dried

실험 절차

3.2 Grams (12 mmol) of 5,8-dimethyl-6-bromothiochroman-4-one and 1.9 g (23 mmol) of O-methylhydroxylamine hydrochloride were refluxed in a solvent mixture of 10 ml of ethanol and 10 ml of pyridine under heat for 30 minutes. The solvent was distilled off under reduced pressure, and then 50 ml of 5% hydrochloric acid was added to form a solid. The solid was recovered by filtration, washed with water and dried to give 3.4 g of 4-methoxyimino-5,8-dimethyl-6-bromothiochroman (yield 93%).

출처