反应详情

CsF (approximately 0.2 g) was added to a mixture of crude 6-chloro-2,4-difluoro-3-(trimethylsilyl)benzaldehyde (10.5 g, approximately 42 mmol) in dimethylformamide (15 mL)/H2O (2 mL). After stirring for 10 min the reaction was diluted with heptane and H2O. The phases were separated and the aqueous extracted with further heptane. The combined organic layers were washed with H2O, dried over MgSO4 and concentrated in vacuo to a yellow oil. Purification by column chromatography (1:4 EtOAc:heptane) followed by trituration with pentane gave the title compound as a white solid (3.0 g, 17.0 mmol).

1. customThe phases were separated
2. extractionthe aqueous extracted with further heptane
3. washThe combined organic layers were washed with H2O
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo to a yellow oil
6. customPurification by column chromatography (1:4 EtOAc:heptane)