反应详情

To a solution of 5-cyano-2-fluorobenzaldehyde (1.50 g, 10.06 mmol) in THF (15 mL) cooled to 0° C. was added methyllithium (7.90 mL, 11.06 mmol). The mixture was stirred at room temperature for 2 h and quenched by the addition of saturated NH4Cl (10 mL). The mixture was partitioned between ethyl acetate (50 mL) and water (20 mL), the organic was washed with water (20 mL), dried over magnesium sulfate and concentrated in vacuo to provide a residue. Purification via flash column chromatography (30×150 mm column; elution with EtOAc: Hex, 1:2) afforded pure compound:

1. customquenched by the addition of saturated NH4Cl (10 mL)
2. customThe mixture was partitioned between ethyl acetate (50 mL) and water (20 mL)
3. washthe organic was washed with water (20 mL)
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated in vacuo
6. customto provide a residue
7. customPurification
8. washvia flash column chromatography (30×150 mm column; elution with EtOAc: Hex, 1:2)
9. customafforded pure compound