反应详情

温度

110 °C

To a solution of intermediate D2 (1.44 g, 8.6 mmol) in DMF (140 ml) was added phosphorus oxybromide (5.4 g, 18.9 mmol) and the mixture was heated at 110° C. for 1 hour. After cooling in an ice bath the solution was partitioned between water and EtOAc. After three extractions with EtOAc the combined organic fractions were dried (Na2SO4) and the solvent evaporated in vacuo. The crude product was purified by column chromatography (silica gel; DCM as eluent). The desired fractions were collected and evaporated in vacuo to yield intermediate D3 (1.82 g, 93%).

1. temperatureAfter cooling in an ice bath the solution
2. customwas partitioned between water and EtOAc
3. extractionAfter three extractions with EtOAc the combined organic fractions
4. dry with materialwere dried (Na2SO4)
5. customthe solvent evaporated in vacuo
6. customThe crude product was purified by column chromatography (silica gel; DCM as eluent)
7. customThe desired fractions were collected
8. customevaporated in vacuo