反应详情

温度

70 °C

A solution of 3-chloro-6,7-dihydro-5H-[1]pyrindine (3.03 g, 19.7 mmol) in acetic acid (19.7 ml) was treated at room temperature with hydrogen peroxide (3.45 ml, 39.5 mmol). The mixture was heated to 70° C. and stirred at this temperature overnight. After completion, the reaction mixture was allowed to cool and was concentrated at reduced pressure. Water was added and the mixture was evaporated again. This procedure was repeated another 2 times. The residue was dissolved in ethyl acetate, washed with a saturated aqueous solution of sodium hydrogen carbonate and brine, then dried over sodium sulfate and evaporated at reduced pressure. The crude 3-chloro-6,7-dihydro-5H-[1]pyrindine 1-oxide was obtained as dark green crystals (2.07 g, 62% yield). MS (ISP): m/z=170 [M+H]+.

1. temperatureto cool
2. concentrationwas concentrated at reduced pressure
3. additionWater was added
4. customthe mixture was evaporated again
5. dissolutionThe residue was dissolved in ethyl acetate
6. washwashed with a saturated aqueous solution of sodium hydrogen carbonate and brine
7. dry with materialdried over sodium sulfate
8. customevaporated at reduced pressure