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
- 50 °C
PROCEDURE
实验过程
To a mixture of 3-(8-(6-(2-methylpyrrolidin-1-yl)pyridin-2-ylamino)imidazo[1,2-b]pyridazin-6-yl)phenol (50 mg, 0.129 mmol) and K2CO3 (36 mg, 0.258 mmol) in DMF (5 mL) was added tert-butyl 4-(2-(methylsulfonyloxy)ethyl)piperazine-1-carboxylate (48 mg, 0.155 mmol). The mixture was heated at 50° C. for 16 h. After cooling, the mixture was poured into water and extracted with EtOAc (3×10 mL). The combined organic layers were washed with brine and dried over MgSO4. After filtration and concentration, the residue was washed by petroleum ether to give tert-butyl-4-(2-(3-(8-(6-(2-methylpyrrolidin-1-yl)pyridin-2-ylamino)imidazo[1,2-b]pyridazin-6-yl)phenoxy)ethyl)piperazine-1-carboxylate (25 mg, 33%) as crude oil. LC-MS: 599.4 [M+H]+, tR=1.53 min.
WORKUP
后处理
- temperatureAfter cooling
- extractionextracted with EtOAc (3×10 mL)
- washThe combined organic layers were washed with brine
- dry with materialdried over MgSO4
- filtrationAfter filtration and concentration
- washthe residue was washed by petroleum ether