反应详情

温度

-55 °C

0.53 ml of diethylaminosulfide trifluoride (DAST) were added at about -60° C. to a solution of 1 g of the product of Stage C and 5 ml of methylene chloride and the reaction mixture was stirred for 2 hours at -55° C. and poured into a solution of sodium bicarbonate. Extraction was carried out with methylene chloride and the extracts were dried over magnesium sulfate, filtered and evaporated to dryness. The residue was taken up in 5 ml of methanol and 20 mg of toluene-sulfonic acid were added. The reaction mixture was stirred for one hour at 20° C., followed by evaporation to dryness. The residue was chromatographed on silica eluting with a hexane-ethyl acetate mixture (7-3) to obtain 0.16 g of the desired product with a Rf=0.10.

1. extractionExtraction
2. dry with materialthe extracts were dried over magnesium sulfate
3. filtrationfiltered
4. customevaporated to dryness
5. addition20 mg of toluene-sulfonic acid were added
6. stirringThe reaction mixture was stirred for one hour at 20° C.
7. customfollowed by evaporation to dryness
8. customThe residue was chromatographed on silica eluting with a hexane-ethyl acetate mixture (7-3)