HRID1159796
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
1-(Phenylsulfonyl)-4-vinyl-1H-indole (190 mg, 0.7 mmol, Intermediate 45) was weight in to a pre dried reaction flask and purged with nitrogen gas for 1 h. Dry THF (50 mL) was added and the reaction flask was cooled to −78° C. before LDA (0.35 mL, 0.7 mmol, 2M) was added. The reaction was stirred for 15 minutes before iodomethane (95.2 mg, 0.7 mmol) was added. Allowed the reaction mixture to slowly reach RT ON. Added 1 mL MeOH and evaporated the reaction mixture on silica. Purified by flash chromatography using 20% DCM in hexanes. Got 61 mg of a white solid, 30% yield. MS (ESI+) for C17H15NO2S m/z 298 (M+H)+.
WORKUP
后处理
- customdried
- customreaction flask
- custompurged with nitrogen gas for 1 h
- additionDry THF (50 mL) was added
- additionwas added
- additionwas added
- customto slowly reach RT
- customevaporated the reaction mixture on silica
- customPurified by flash chromatography