反应详情

温度

12 °C

A mixture of compound 2,3,4,5-tetrahydro-2,8-dimethyl-1H-pyrido[4,3-b]indole (1.5 g, 7.5 mmol, 1 equiv.) and NaH (252 mg, 10.5 mmol, 1.4 equiv) in 30 ml of DMF were heated to 12° C., 1 h. It was cooled to RT and compound 2-methyl-5-(2-methyloxiran-2-yl)pyridine (2.46 g, 16.5 mmol, 2.2 equiv) in 17 ml DMF was added dropwise over 12 min. The temperature was again raised to 120 deg C. and stirred for 3 h. The reaction mixture was cooled to RT and 5 ml of water was added to it, diluted with 700 ml of ethyl acetate and the organic part was washed with water (100 ml×3) and then with brine. It was dried over sodium sulphate and concentrated under vacuum. Column purified over 230-400 silica gel using a gradient of 10-20% methanol in ethyl acetate. Yield: 2.3 g (87%)

1. temperatureIt was cooled to RT
2. temperatureThe temperature was again raised to 120 deg C
3. temperatureThe reaction mixture was cooled to RT
4. washthe organic part was washed with water (100 ml×3)
5. dry with materialIt was dried over sodium sulphate
6. concentrationconcentrated under vacuum
7. customColumn purified over 230-400 silica gel using a gradient of 10-20% methanol in ethyl acetate