HRID1515496

反应详情

EQUATION

反应方程式

HRID 1515496 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

A mixture of 3-aminobenzamide (204 mg, 1.5 mmol), 3,4-dimethoxyphenylboronic acid (273 mg, 1.5 mmol) and glyoxylic acid monohydrate (138 mg, 1.5 mmol) in acetonitrile (8.0 mL) and DMF (0.8 mL) was heated at 55° C. for 4.0 h and then stirred at rt for 18 h. The precipitate formed was collected by filtration and washed with ethyl acetate to give 1A (390 mg, 78% yield) after drying. 1H NMR (400 MHz, DMSO-d6) δ ppm 7.03-7.19 (m, 5H) 6.91 (d, J=9.0 Hz, 1H) 6.81 (d, J=8.00 Hz, 1H) 5.05 (s, 1H) 3.83 (s, 3H) 3.72 (s, 3H). LC-MS 331 (M+H).

WORKUP

后处理

  1. customThe precipitate formed
  2. filtrationwas collected by filtration
  3. washwashed with ethyl acetate