反应详情

温度

230 °C

A mixture of 40 parts of methyl 4-(acetylamino)-5-chloro-2-(2-propynoxy)benzoate and 172 parts of phenoxybenzene was stirred for 45 min. at 230° C. After cooling, the reaction mixture was poured into petroleumether. The organic layer was separated, dried, filtered and evaporated. The residue was purified by column chromatography (silica gel; CH2Cl2 /CH3OH 97:3). The eluent of the desired fractions was evaporated and the residue was crystallized from acetonitrile, yielding 11.9 parts (33.8%) of methyl 5-(acetylamino)-6-chloro-2H-1-benzopyran-8-carboxylate (interm 11).

1. temperatureAfter cooling
2. additionthe reaction mixture was poured into petroleumether
3. customThe organic layer was separated
4. customdried
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by column chromatography (silica gel; CH2Cl2 /CH3OH 97:3)
8. customThe eluent of the desired fractions was evaporated
9. customthe residue was crystallized from acetonitrile