反应详情

To a solution of Intermediate 350B (1.1 g, 3.05 mmol) in THF (10 mL) was added BH3.DMS (0.578 mL, 6.09 mmol, 2M) and the resulting solution was stirred at 40° C. for 18 h. The reaction mixture was cooled to RT, quenched with ethanol (10 mL) and heated to reflux for 1 h. Reaction mixture was concentrated under reduced pressure. The crude product was purified by silica gel chromatography (24 g REDISEP® column, eluting with 2% MeOH in CHCl3). Fractions containing the product were combined and evaporated to afford Intermediate 350C (0.7 g, 66%) as a gummy solid. MS(ES): m/z=348 [M+H]+.

1. customquenched with ethanol (10 mL)
2. temperatureheated
3. temperatureto reflux for 1 h
4. customReaction mixture
5. concentrationwas concentrated under reduced pressure
6. customThe crude product was purified by silica gel chromatography (24 g REDISEP® column, eluting with 2% MeOH in CHCl3)
7. additionFractions containing the product
8. customevaporated