反应详情

温度

110 °C

Palladium tetrakis(triphenylphosphine) (169 mg, 0.15 mmol) was added to a degassed, ambient temperature solution of 1-tert-butyl 2-methyl 2-(4-bromobenzyl)-4,4-difluoropyrrolidine-1,2-dicarboxylate (634 mg, 1.46 mmol), 2-bromo-5-fluoropyridine (257 mg, 1.46 mmol), and hexamethylditin (478 mg, 1.46 mmol) in 1,4-dioxane (5 mL). After stirring at 110° C. overnight, potassium fluoride (50% on celite) was added. After stirring vigorously for a further 1 h, the reaction mixture was filtered, washed with water, dried (magnesium sulfate), filtered and concentrated in vacuo. Chromatography over silica eluting with 0-50% ethyl acetate/hexane afforded 1-tert-butyl 2-methyl 4,4-difluoro-2-[4-(5-fluoropyridin-2-yl)benzyl]pyrrolidine-1,2-dicarboxylate.

1. stirringAfter stirring vigorously for a further 1 h
2. filtrationthe reaction mixture was filtered
3. washwashed with water
4. dry with materialdried (magnesium sulfate)
5. filtrationfiltered
6. concentrationconcentrated in vacuo