反应详情

The crude methyl 2-amino-2-(furan-2-yl)acetate (Example 2c) was dissolved in 350 mL of anhydrous ether and with rapid magnetic stirring, 10 mL of 33% wt HBr in acetic acid was added slowly by syringe. After stirring for 30 min, filtration followed by air drying gave methyl 2-amino-2-(furan-2-yl)acetate hydrobromide (12.35 g, 51.8 mmol, 54.2% yield) as an off-white solid; Mp 141-142° C. 1H NMR (400 MHz, DMSO-d6) δ 8.84 (s, 2H), 7.81 (dd, J=1.8, 0.7 Hz, 1H), 5.68 (d. J=3.3 Hz, 1H), 6.56 (dd, =3.3, 1.9 Hz, 1H), 5.59 (s, 1H), 3.77 (s, 3H); 13C NMR (151 MHz, DMSO-d6) δ 167.44, 145.49, 145.06, 112.14, 111.70, 53.98, 49.73.

1. additionwas added slowly by syringe
2. filtrationfiltration
3. customdrying