反应详情

温度

-78 °C

0.11 ml of DAST is added dropwise to a solution of 0.1 g of the compound obtained in Step 14.3 in 2 ml of DCM cooled to −78° C. The reaction medium is stirred for 2 hours at −78° C. and then allowed to warm to room temperature. It is neutralized with saturated NaHCO3 solution. The resulting mixture is extracted with DCM. The organic phase is dried over Na2SO4, filtered and evaporated under reduced pressure. The residue is chromatographed on silica gel, eluting with a DCM/EtOAc mixture from (95/5, v/v) to (30/70, v/v) to give 0.032 g of the expected product.

1. temperatureto warm to room temperature
2. extractionThe resulting mixture is extracted with DCM
3. dry with materialThe organic phase is dried over Na2SO4
4. filtrationfiltered
5. customevaporated under reduced pressure
6. customThe residue is chromatographed on silica gel
7. washeluting with a DCM/EtOAc mixture from (95/5