HRID69157

反应详情

EQUATION

反应方程式

HRID 69157 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

The compound 6-chloro-3-(4-methoxy-benzyl)-imidazo-[1,2-b]-pyridazine (Stage 4.1, 100 mg, 0.36 mmol) was introduced in a microwave reactor with 1-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaboran-2-yl)-1H-pyrazole (75 mg, 0.36 mmol) and dissolved in 1 mL of 2-dimethoxyethane. An aqueous solution of 2 M Na2CO3 (660 μL, 1.3 mmol) was added to this mixture and also tetrakis-(triphenylphosphine)-palladium (21 mg, 0.02 mmol). The RM was heated at 180° C. for 30 min under microwave irradiations. The reaction was taken up with EtOAc and washed with 10% Na2CO3 and brine. The organic layer was dried over Na2SO4 and the solvent was removed. The residue was purified by preparative HPLC with acetonitrile and water (+0.1% TFA). The white solid the title compound was obtained (tR 1.0 min (conditions 2), MH+=320).

WORKUP

后处理

  1. washwashed with 10% Na2CO3 and brine
  2. dry with materialThe organic layer was dried over Na2SO4
  3. customthe solvent was removed
  4. customThe residue was purified by preparative HPLC with acetonitrile and water (+0.1% TFA)