反应详情

温度

-15 °C

mL ethyl magnesium bromide solution (191.8 mmol, 1.10 eq) were diluted with 182.6 mL diethylether. The solution was cooled to −15° C. and a solution of 30.20 g of compound (8) as obtained from example 1 (174.4 mmol) in 60.4 mL diethylether was added dropwise. The resulting viscous suspension was stirred for additional 75 min at −15° C. Subsequently, the reaction was quenched by addition of 14.96 mL acetic acid (261.6 mmol, 1.5 eq). Then, 35 mL water were added to dissolve all salts and the cooling bath was removed. After 15 min, the mixture was washed twice with 200 mL, pH-7-buffer and the organic phase was dried over 20 g sodium sulfate and was filtered. The filter cake was washed with 40 mL diethylether. After evaporation of solvent in a rotary evaporator (40° C./10 mbar), the crude product (26.33 g, 96% by weight) was obtained as a yellow liquid. Purification was achieved using a high vacuum distillation (bp 86° C. at 2.5 mbar) furnishing the title compound (18.66 g, 118.7 mmol, 68% by weight) as colorless liquid.

1. additionwas added dropwise
2. dissolutionto dissolve all salts
3. customthe cooling bath was removed
4. waitAfter 15 min
5. washthe mixture was washed twice with 200 mL, pH-7-buffer and the organic phase
6. dry with materialwas dried over 20 g sodium sulfate
7. filtrationwas filtered
8. washThe filter cake was washed with 40 mL diethylether
9. customAfter evaporation of solvent
10. customin a rotary evaporator (40° C./10 mbar)
11. customthe crude product (26.33 g, 96% by weight) was obtained as a yellow liquid
12. customPurification
13. distillationa high vacuum distillation (bp 86° C. at 2.5 mbar)