反应详情

温度

60 °C

19.5 g (170 mmol) of tert-butyl nitrite 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 then stirred at 60° C. for 1.5 hours. For work-up, the solid is filtered off with suction and the solution is diluted with methylene chloride and extracted with dilute hydrochloric acid. The organic phase is washed with saturated aqueous NaHCO3 solution, dried over sodium sulfate, filtered off and concentrated. Excess dimethyl disulfide is removed under oil pump vacuum.

1. filtrationFor work-up, the solid is filtered off with suction
2. additionthe solution is diluted with methylene chloride
3. extractionextracted with dilute hydrochloric acid
4. washThe organic phase is washed with saturated aqueous NaHCO3 solution
5. dry with materialdried over sodium sulfate
6. filtrationfiltered off
7. concentrationconcentrated
8. customExcess dimethyl disulfide is removed under oil pump vacuum