反应详情

温度

-30 °C

To a solution of intermediate 1g (200 mg, 0.519 mmol) in 5 mL THF at −78° C., was added a 1M solution of LIHMDS in THF (1.09 mL, 1.09 mmol). The mixture was stirred for 5 min, then MeI (162 mL, 2.60 mmol) was added. The mixture was stirred with warming to −30° C. over 1 h, then was quenched with sat. NH4Cl. The mixture was diluted with EtOAc and washed with H2O and brine, dried (Na2SO4), and concentrated. The resultant residue was combined with additional crude material from another batch for purification by flash chromatography (stepwise gradient, 40 to 45 to 50% EtOAc/hexanes) to afford 59 mg of intermediate 19a (18%, based on 0.835 mmol of starting material). LR MS.

1. stirringThe mixture was stirred
2. customwas quenched with sat. NH4Cl
3. additionThe mixture was diluted with EtOAc
4. washwashed with H2O and brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customThe resultant residue was combined with additional crude material from another batch for purification by flash chromatography (stepwise gradient, 40 to 45 to 50% EtOAc/hexanes)