反应详情

温度

55 °C

A mixture of methyl 2,2-dimethoxypropionate (2.33 g, 15.7 mmol) and benzylamine (1.68 g, 15.7 mmol) in a 20 mL screw-capped vial was stirred at 55° C. for 12 d. To the reaction mixture, which mostly solidified upon cooling to ambient temperature was added hexane (5 mL), and the mixture was sonicated and stirred vigorously. The solid was filtered off, washed with hexanes, and dried in vacuo to give the title compound as off-white solid. 1H NMR (400 MHz, CDCl3): δ=7.38-7.25 (m, 5H), 7.08 (brs, 1H), 4.49 (d, J=5.6 Hz, 2H), 3.25 (s, 6H), 1.52 (s, 3H). MS(ES+): m/z=246.07 (58) [MNa+], 224.11 (58) [MH+], 192.12 (100) [MH+-MeOH], 160.11 (33) [MH+-2 MeOH]. HPLC: tR=2.78 min (polar—5 min, ZQ3).

1. customscrew-capped vial
2. temperatureupon cooling to ambient temperature
3. customthe mixture was sonicated
4. stirringstirred vigorously
5. filtrationThe solid was filtered off
6. washwashed with hexanes
7. customdried in vacuo