반응 #77942

반응 방정식

tert-butylnitrite

dimethyl disulfide

2-(4,5-dihydroisoxazol-3-yl)-3-methylaniline

dimethyl disulfide

→

3-(2-methyl-6-methylthiophenyl)-4,5-dihydroisoxazole

반응 조건

후처리

1. 1
   여과For work-up, the solid is filtered off with suction
2. 2
   workup.ADDITIONthe filtrate is diluted with methylene chloride
3. 3
   추출extracted with dilute hydrochloric acid
4. 4
   세척The organic phase is washed with saturated aqueous NaHCO3 solution
5. 5
   건조dried over sodium sulfate
6. 6
   여과the drying agent is filtered off
7. 7
   농축the filtrate is concentrated
8. 8
   기타Excess dimethyl disulfide is removed under oil pump vacuum

실험 절차

19.5 g (170 mmol) of tert-butylnitrite and 20 g of copper powder are initially charged in 30 ml of dimethyl disulfide, and a solution of 20 g (114 mmol) of 2-(4,5-dihydroisoxazol-3-yl)-3-methylaniline in 100 ml of dimethyl disulfide is added dropwise at from 50 to 55° C. The mixture is subsequently stirred at 60° C. for 1.5 hours. For work-up, the solid is filtered off with suction, and the filtrate is diluted with methylene chloride and extracted with dilute hydrochloric acid. The organic phase is washed with saturated aqueous NaHCO3 solution and dried over sodium sulfate, the drying agent is filtered off and the filtrate is concentrated. Excess dimethyl disulfide is removed under oil pump vacuum.

출처