反应详情

TEA (3.705 g, 36.619 mmol) was added to a solution of methyl 2-mercaptoacetate (3.293 g, 30.985 mmol) in CH3CN (12.5 mL). This was followed by the addition of 2,5-difluorobenzaldehyde (4 g, 28.169 mmol) in CH3CN (12.5 mL) and the resulting reaction mass was refluxed overnight under nitrogen atmosphere. The reaction was monitored by TLC (5% ethyl acetate in hexane). The reaction mass was concentrated under reduced pressure to obtain the crude product. Purification by column chromatography on silica gel (15% ethyl acetate in hexane) afforded 2 g of the product (33.89% yield).

1. customthe resulting reaction mass
2. temperaturewas refluxed overnight under nitrogen atmosphere
3. concentrationThe reaction mass was concentrated under reduced pressure
4. customto obtain the crude product
5. customPurification by column chromatography on silica gel (15% ethyl acetate in hexane)