HRID1755377
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
- 100 °C
PROCEDURE
实验过程
A mixture of methyl 3-(8-bromoimidazo[1,2-b]pyridazin-6-yl)benzoate (0.2 g, 0.6 mmol), 6-(2,5-dimethylpyrrolidin-1-yl)pyridin-2-amine (116 mg, 0.6 mmol), Pd2(dba)3 (0.036 g, 0.06 mmol), BINAP (0.076 g, 0.12 mmol) and Cs2CO3 (0.59 g, 1.8 mmol) in dioxane (5 mL) was heated to 100° C. for 15 h in a sealed tube under N2 atmosphere then concentrated in vacuo. The residue was purified by chromatography (silica gel, 10 g, 200˜300 mesh, dichloromethane:MeOH=100:1) to afford methyl 3-(8-(6-(2,5-dimethylpyrrolidin-1-yl)pyridin-2-ylamino)imidazo[1,2-b]pyridazin-6-yl)benzoate (150 mg, 56%) as a brown solid. LC-MS: [M+1]+=443, tR=2.092 min.
WORKUP
后处理
- concentrationthen concentrated in vacuo
- customThe residue was purified by chromatography (silica gel, 10 g, 200˜300 mesh, dichloromethane:MeOH=100:1)