反应详情

温度

-30 °C

A solution of the product from Example 2a (7.53 g, 40.0 mmol) in 30 mL of dry THF was added dropwise with stirring to a solution of LDA (42.4 mmol) in 30 mL of dry THF at −30° C. Stirred at −30° C. for 30 min. Added EtI (3.42 mL, 42.0 mmol) in 20 mL of dry THF dropwise with stirring for 30 min then warmed to room temperature. After 2 h quenched by pouring into saturated NaCl solution and extracted with ether. Dried over MgSO4, filtered and concentrated under vacuum giving the title compound. The product was purified by silica gel column chromatography eluting with EtOAc/hexane to give the title compound (5.21 g, 60%).

1. temperaturethen warmed to room temperature
2. customAfter 2 h quenched
3. additionby pouring into saturated NaCl solution
4. extractionextracted with ether
5. dry with materialDried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated under vacuum