反应详情

温度

-10 °C

Analogously to example I, 2-lithium-2-butene was prepared from 2-bromo-2-butene (15.0 g; 0.11 mol) and lithium (2.8 g; 0.26 mol). To the product obtained, ethyl 4-bromobutanoate (11.0 g; 0.056 mol) was added dropwise and with reflux at -40-20° C., followed by stirring for 30 minutes at -20° C. Water (200 ml) and subsequently pentane (100 ml) were slowly added dropwise at -20° C. After separation of the layers the water layer was washed two times with 100 ml of pentane/ether (1/1, v/v), after which the combined organic layers were washed with water (50 ml). The organic layer was dried (K2CO3), filtered and evaporated. The yield was 14.0 g (96%).

1. customTo the product obtained
2. customAfter separation of the layers the water layer
3. washwas washed two times with 100 ml of pentane/ether (1/1
4. washv/v), after which the combined organic layers were washed with water (50 ml)
5. dry with materialThe organic layer was dried (K2CO3)
6. filtrationfiltered
7. customevaporated