反应详情

温度

0 °C

Under argon, 7.6 g (23.3 mmol) of the compound of Example 15A were dissolved in 76 ml of THF, and a few granules of 4 Å molecular sieve were added. The mixture was then cooled to 0° C., and 53.7 ml (69.8 mmol) of a 1.3 M solution of 2-propylmagnesium chloride/lithium chloride complex in THF were slowly added dropwise. After the addition had ended, the reaction mixture was stirred at 0° C. for another 30 min. 2.6 ml (34.9 mmol) of anhydrous acetone were then added, and the reaction was stirred at 0° C. for another 1 h. 90 ml of 1 M hydrochloric acid were then added, and the reaction was allowed to slowly warm to RT over a period of 40 min. The mixture was then extracted three times with ethyl acetate. The combined organic phases were washed with saturated sodium chloride solution, dried over sodium sulphate, filtered and concentrated. The residue was triturated with petroleum ether with a little diethyl ether added, filtered off and dried. This gave 5.8 g (80% of theory) of the title compound as a white solid.

1. additiona few granules of 4 Å molecular sieve were added
2. additionAfter the addition
3. stirringthe reaction was stirred at 0° C. for another 1 h
4. temperatureto slowly warm to RT over a period of 40 min
5. extractionThe mixture was then extracted three times with ethyl acetate
6. washThe combined organic phases were washed with saturated sodium chloride solution
7. dry with materialdried over sodium sulphate
8. filtrationfiltered
9. concentrationconcentrated
10. customThe residue was triturated with petroleum ether with a little diethyl ether
11. additionadded
12. filtrationfiltered off
13. customdried