反应详情

To a stirred solution of 2-amino-3-(hydroxymethyl)pyridine (113a) (156 g, 1.257 mole) in HOAc (2.5 L) at ambient temperature was added bromine (64.1 mL, 1.257 mole) dropwise over 1 hr. A suspension began to form during the addition. An exotherm to 36° C. was controlled with an ice bath. After the addition, the reaction mixture was stirred at ambient temperature overnight. The yellow precipitate was filtered, washed with ether and air-dried to give the title compound (289 g, 81%): MS (ES) m/e 203.2 (M+H)+; 1H NMR (400 MHz, DMSO-d6, free base) δ 7.89 (d, J=2.3 Hz, 1H), 7.52 (s, 1H), 5.92 (br s, 2H), 5.29 (br s, 1H), 4.30 (s, 2H).

1. customto form during the addition
2. customAn exotherm to 36° C. was controlled with an ice bath
3. additionAfter the addition
4. filtrationThe yellow precipitate was filtered
5. washwashed with ether
6. customair-dried