HRID2357532
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture was cooled to RT
- custompurified by flash chromatography (silica gel)
- washeluting with 2% 2 M ammonia in MeOH/DCM to 6% 2 M ammonia MeOH/DCM