HRID2357675

反应详情

EQUATION

反应方程式

HRID 2357675 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

This compound was prepared by a method analogous to that described in Example 8 (Method A). A mixture of 4-(6-bromophthalazin-1-yl)-3-methylpiperazin-2-one (0.200 g, 0.62 mmol), N-cyclopropyl-4-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzamide (0.245 g, 0.81 mmol), sodium carbonate (0.270 g, 2.5 mmol) and trans-dichlorobis(triphenyl-phosphine)palladium (II) (0.040 g, 0.050 mmol) in DME (7 mL)/H2O (3 mL)/EtOH (2 mL) was heated at 90° C. The reaction was purified by flash chromatography eluting with 2M NH3 in MeOH/CH2Cl2 (0:1-1:19) to give 126 mg of a brown amorphous solid. The material was further purified by reverse phase HPLC (10→100% CH3CN [0.1% TFA]) to give the title compound as a light yellow amorphous solid. Found MS m/z: 416.2 [M+1].

WORKUP

后处理

  1. customThis compound was prepared by a method analogous to
  2. customThe reaction was purified by flash chromatography
  3. washeluting with 2M NH3 in MeOH/CH2Cl2 (0:1-1:19)