HRID2357583
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
- 90 °C
PROCEDURE
实验过程
A mixture of 4-(6-bromophthalazin-1-yl)piperazin-2-one (0.10 g, 326 μmol), N-cyclopropyl-4-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzamide (98mg, 326 μmol), and tetrakis(triphenylphosphine)palladium (19 mg, 16 μmol) in 5 mL DME/EtOH (4:1) was treated with 2M potassium carbonate (488 μl, 977 μmol). The resulting mixture was warmed up to 90° C. and stirred for 1 h under nitrogen. The mixture was cooled to room temperature, and the crude product was purified via flash chromatography (silica gel) eluting with a gradient of 4% 2 M ammonia in MeOH/DCM to 6% 2 M ammonia in MeOH/DCM to give the title compound (0.11 g) as a pale yellow solid. Found MS(ES+): 402(M+H)+.
WORKUP
后处理
- temperatureThe mixture was cooled to room temperature
- customthe crude product was purified via flash chromatography (silica gel)
- washeluting with a gradient of 4% 2 M ammonia in MeOH/DCM to 6% 2 M ammonia in MeOH/DCM