反应详情

To the solution of para formaldehyde (9.6 g, 319.55 mmol) and sodium ethoxide (0.87 g, 12.784 mmol) in dry THF (250 ml) was added (6-bromo-pyridin-2-yl)-acetic acid ethyl ester (31.2 g, 127.82 mmol) at 0° C. to −10° C. and allowed the reaction mixture to stir at same temperature for 4 h. Solids formed in the reaction mixture were filtered and washed with ethyl acetate and the filtrate was concentrated to obtain crude product as a brown liquid. Yield=30.0 g (crude). TLC (30% ethyl acetate in hexane) Rf=0.28; LCMS: RtH8=0.702, M+1=304.0 and 306.0.

1. customSolids formed in the reaction mixture
2. filtrationwere filtered
3. washwashed with ethyl acetate
4. concentrationthe filtrate was concentrated
5. customto obtain crude product as a brown liquid