HRID643950

反应详情

EQUATION

反应方程式

HRID 643950 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 7-benzyloxy-3-methoxy-6-nitrochromen-2-one (0.20 g, 0.61 mmol) in 20 mL of THF is added a solution of Na2S2O4 (1.0 g) in water (6 mL). The mixture is heated at 80° C. for 18 h. Additional Na2S2O4 is added until the reaction is complete. After cooling to ambient temperature, EtOAc is added and the mixture is washed with water and sat. NaCl, then dried over sodium sulfate. The solvent is removed under reduced pressure to afford 6-amino-7-benzyloxy-3-methoxychromen-2-one as a pale yellow solid: 1H NMR (CDCl3) δ 7.44-7.34 (m, 5H), 6.81 (s, 1H), 6.70 (s, 1H), 6.68 (s, 1H), 5.11 (s, 2H), 3.85 (s, 3H); (M+H)+=298.

WORKUP

后处理

  1. temperatureAfter cooling to ambient temperature
  2. washthe mixture is washed with water and sat. NaCl
  3. dry with materialdried over sodium sulfate
  4. customThe solvent is removed under reduced pressure