反应详情

温度

-78 °C

To a stirred solution of 36-1 (0.46 g, 1.38 mmol) in THF (8 mL) chilled to −78° C. was added DIBAL 1.0M in THF heptane (4.22 mL, 4.22 mmol) dropwise. The resulting mixture was stirred at −78° C. for 3 hr, then quench with slow addition of Rochelle's salt solution (5 mL). The resulting mixture was allowed to warm to room temperature, diluted with water and extracted with ethyl acetate. The organic phase was concentrated and flash column separation using a 50-100% ethyl acetate/hexane gradient gave 36-2. (0.26 g, 64%). LRMS (ES) (M+H)+: observed=292.1, calculated=292.4.

1. customquench with slow addition of Rochelle's salt solution (5 mL)
2. temperatureto warm to room temperature
3. additiondiluted with water
4. extractionextracted with ethyl acetate
5. concentrationThe organic phase was concentrated
6. customflash column separation
7. customgave 36-2