反应详情

温度

10 °C

To a cold solution of crude 1261-B (109 mmol) in DMF (90 ml) was added Potassium thioacetate (1.2 equiv, 131 mmol, 15 g) maintaining temperature below 30° C. The reaction was stirred for 18 h then cooled to 10° C. and water (160 mL) was added. Reaction was extracted with EtOAc and washed with NaHCO3 sat., then brine. The dark organic layer was dried over MgSO4, filtered and concentrated down to a dark oil. Purification—HPFC (High Pressure Flash Chromatography) 75+M prepacked silica cartridge (1 to 5% EtOAc), UV collection. After concentration, 20.43 g of product 1261-C was obtained.

1. temperaturemaintaining temperature below 30° C
2. customReaction
3. extractionwas extracted with EtOAc
4. washwashed with NaHCO3 sat.
5. dry with materialThe dark organic layer was dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated down to a dark oil
8. customPurification—HPFC (High Pressure Flash Chromatography) 75+M prepacked silica cartridge (1 to 5% EtOAc), UV collection
9. concentrationAfter concentration