HRID347536

反应详情

EQUATION

反应方程式

HRID 347536 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 6-phenylpicolinic acid (150 mg, 0.75 mmol), K2HPO4 (600 mg) m-CPBA (300 mg, max 70% from Aldrich) in dichloroethane (8.0 mL) was heated at 60° C. for 1.5 h. Additional m-CPBA (2×300 mg) was added and the mixture was heated at 60° C. for 40 min. The reaction mixture was purified by preparative HPLC to afford the desired product (110 mg, 68%) as a white solid. 1H NMR (DMF-d7) δ 8.57 (s, 1H), 8.43 (d, 1H, J=2.2 Hz), 8.10–7.88 (m, 5H), 7.59–7.57 (m, 3H).

WORKUP

后处理

  1. temperaturethe mixture was heated at 60° C. for 40 min
  2. customThe reaction mixture was purified by preparative HPLC