HRID1690326

反应详情

EQUATION

反应方程式

HRID 1690326 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Bromine (0.7 mL, 14 mmole) was added dropwise to a stirred solution of methyl 2-aminonicotinate (2.0 g, 13 mmole) in HOAc (50 mL). A suspension formed within 30 min. The reaction was allowed to stir at room temperature for 2 h, then was concentrated under vacuum. The residue was triturated with 1.0 N Na2CO3 (50 mL) and the solid was collected by suction filtration. The solid was washed with H2O (50 mL) and dried under vacuum to give the title compound (2.95 g, 98%) as a pale yellow solid: 1H NMR (400 MHz, CDCl3) δ 8.24 (d, J=2.5 Hz, 1 H), 8.23 (d, J=2.5 Hz, 1 H), 6.40 (br s, 2 H), 3.90 (s, 3 H).

WORKUP

后处理

  1. customA suspension formed within 30 min
  2. concentrationwas concentrated under vacuum
  3. customThe residue was triturated with 1.0 N Na2CO3 (50 mL)
  4. filtrationthe solid was collected by suction filtration
  5. washThe solid was washed with H2O (50 mL)
  6. customdried under vacuum