反应详情

温度

-70 °C

3-Cyano-4-fluorobenzaldehyde (2.17 g, 14.7 mmol) was dissolved in THF (50 mL) then cooled to −70° C. To this mixture was added methyl magnesiumbromide (5.34 mL, 16.0 mmol). The mixture was stirred for 1 h, then was quenched with brine and extracted with ether. The ethereal layer was separated, dried over Na2SO4, filtered, and evaporated to dryness. The residue was purified by MPLC chromatography through a 120 g Redi-sep column using 0-50% EtOAc/hexane eluent to yield 2-fluoro-5-(1-hydroxyethyl)benzonitrile: LC-MS: M+1=166.

1. customwas quenched with brine
2. extractionextracted with ether
3. customThe ethereal layer was separated
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. customevaporated to dryness
7. customThe residue was purified by MPLC chromatography through a 120 g Redi-sep column