反应详情

温度

0 °C

2.00 g (10.86 mmol) of the compound from Example 170A were dissolved in 40 ml of diethyl ether at 0° C., and 5.4 ml (16.29 mmol) of a 3N solution of methylmagnesium bromide in diethyl ether were slowly added dropwise. Stirring at 0° C. for 1 h was followed by warming to RT, addition of water and diethyl ether to the reaction solution and separation of the phases. The aqueous phase was extracted with diethyl ether, and the combined organic phases were dried over sodium sulfate and filtered, and the solvents were removed in vacuo. The crude product was purified by flash chromatography on silica gel (mobile phase: dichloromethane). 2.03 g (93% of theory) of the title compound were obtained.

1. temperatureby warming to RT
2. customto the reaction solution and separation of the phases
3. extractionThe aqueous phase was extracted with diethyl ether
4. dry with materialthe combined organic phases were dried over sodium sulfate
5. filtrationfiltered
6. customthe solvents were removed in vacuo
7. customThe crude product was purified by flash chromatography on silica gel (mobile phase: dichloromethane)