反应详情

温度

0 °C

Potassium carbonate (38.8 g, 281 mmol) is added to 3-bromophenacyl bromide (60 g 216 mmol) in acetonitrile (430 mL), and the mixture is cooled under nitrogen to 0° C. Diallylamine (34.6 mL, 280.63 mmol) is added drop wise over 1 hour and the reaction is allowed to warm to 22° C. overnight. The crude reaction mixture is concentrated and the residue is partitioned in water (300 mL) and MTBE (300 mL). The aqueous layer is discarded and the organic layer is washed with water (100 mL, 2×) and with brine (100 mL). The organic layer is dried over sodium sulfate, filtered, and the solvent evaporated to constant weight to give the title compound (62 g, 98%). ES/MS (m/e): 294 (M+1).

1. temperatureto warm to 22° C. overnight
2. customThe crude reaction mixture
3. concentrationis concentrated
4. customthe residue is partitioned in water (300 mL)
5. washthe organic layer is washed with water (100 mL, 2×) and with brine (100 mL)
6. dry with materialThe organic layer is dried over sodium sulfate
7. filtrationfiltered
8. customthe solvent evaporated to constant weight