反应详情

温度

25 °C

Benzyl alcohol (5.51 mL) was added dropwise over 20 min to a stirred suspension of sodium hydride (2.128 g of a 60% dispersion in mineral oil) and 2,3-difluorobenzonitrile (7.4 g) in THF (100 mL) with external ice bath cooling to maintain temperature around 25° C. After addition was complete, the reaction mixture was stirred at room temperature for 24 h, quenched with water (200 mL) and extracted into ethyl acetate (3×120 mL), combined organics were dried (MgSO4) and evaporated. The residual oil was purified (SiO2 chromatography eluting with 20% ether in isohexane) to give the subtitle compound as an oil (9.70 g).

1. temperaturecooling
2. additionAfter addition
3. customquenched with water (200 mL)
4. extractionextracted into ethyl acetate (3×120 mL)
5. dry with materialcombined organics were dried (MgSO4)
6. customevaporated
7. customThe residual oil was purified
8. wash(SiO2 chromatography eluting with 20% ether in isohexane)