HRID1506002

反应详情

EQUATION

反应方程式

HRID 1506002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A degassed mixture of 3-bromo-9H-dipyrido[2,3-b;4′,3′-d]pyrrole-6-carboxylic acid (20.0 mg, 68.5 μmol), 3-(trifluoromethyl)phenylboronic acid (19.5 mg, 0.103 mmol), and bis(triphenylphosphine)palladium(II) dichloride (2.4 mg, 3.4 μmol) in acetonitrile (0.3 mL) and 2N aqueous sodium carbonate solution (0.3 mL) was heated under microwave irradiation at 140° C. for 10 minutes. The cooled reaction mixture was acidified with 10% aqueous sulfuric acid. The solid was removed by filtration and the resultant filtrate was purified by preparative HPLC (5-45% MeCN over 45 min, 35 mL/min) to afford the title compound. 1H NMR (DMSO-D6, 400 MHz): 12.75 (s, 1H), 9.38-9.00 (m, 311), 8.21 (m, 1H), 7.78 (m, 2H), 7.65-7.60 (m, 2H). LCMS (Method D): RT=10.76 min, M+H+=358.

WORKUP

后处理

  1. customThe cooled reaction mixture
  2. customThe solid was removed by filtration
  3. customthe resultant filtrate was purified by preparative HPLC (5-45% MeCN over 45 min, 35 mL/min)