反应详情

温度

80 °C

A mixture of 382 mg (1 mmole) 4-(2-bromo-6-pyrrolidine-1-yl-pyridine-4-sulfonyl)-phenylamine, 371 mg (1 mmole) tributyl-cyclohex-1-enyl stannane, and 70 mg bis(triphenylphosphine)-palladium(II)-chloride in 20 ml dimethylformamide is stirred for 3 hours at 80° C. The solvent is removed and the residue is diluted with dichloromethane. The dichloromethane solution is washed twice with saturated aqueous potassium fluoride, dried over magnesiumsulfate and concentrated in vacuo. Flash chromatography of the residue (silicagel, hexane/AcOEt 3/1) yields 191 mg (50%) pure 4-(2-cyclohex-1-enyl-6-pyrrolidine-1-yl-pyridine-4-sulfonyl)-phenylamine as a white solid. mp 237-238° C.

1. customThe solvent is removed
2. additionthe residue is diluted with dichloromethane
3. washThe dichloromethane solution is washed twice with saturated aqueous potassium fluoride
4. dry with materialdried over magnesiumsulfate
5. concentrationconcentrated in vacuo