HRID2357532

反应详情

EQUATION

反应方程式

HRID 2357532 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

A mixture of 3-(1-chlorophthalazin-6-yl)-N-cyclopropyl-4-methylbenzamide (63 mg, 212 μmol) (obtained by method C below), 2-chlorophenylboronic acid (40 mg, 254 μmol) and tetrakis(triphenylphosphine)palladium (12 mg, 11 μmol) in DME/ethanol (4:1) (5 mL) was treated with 2 M aq. potassium carbonate (317 μl, 635 μmol). The mixture was warmed to 85° C. and stirred for 3 h. The mixture was cooled to RT and purified by flash chromatography (silica gel) eluting with 2% 2 M ammonia in MeOH/DCM to 6% 2 M ammonia MeOH/DCM to give N-cyclopropyl-4-methyl-3-(1-o-tolylphthalazin-6-yl)benzamide. MS (ES+): 394 (M+H)+.

WORKUP

后处理

  1. temperatureThe mixture was cooled to RT
  2. custompurified by flash chromatography (silica gel)
  3. washeluting with 2% 2 M ammonia in MeOH/DCM to 6% 2 M ammonia MeOH/DCM