HRID710068
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 sealed tube was charged with a mixture prepared by adding toluene (2 ml) to Compound 18 (30 mg), 4-bromopyridazine hydrobromide (22 mg), Pd(OAc)2 (2 mg), Cs2CO3 (37 mg), and [1,1′-binaphthalen]-2-yldi-tert-butylphosphine (3 mg) and the mixture was stirred at 100° C. for 4 hours. After cooling the reaction mixture to room temperature, NH silica gel was added, followed by stirring for a while. After separating the silica gel by filtration, the silica gel was washed with chloroform and the solvent was distilled off; the resulting residue was purified by reverse-phase preparative HPLC to give the titled compound (6.0 mg, colorless oil.)
WORKUP
后处理
- additionA sealed tube was charged with a mixture
- customprepared
- temperatureAfter cooling the reaction mixture to room temperature
- additionNH silica gel was added
- stirringby stirring for a while
- customAfter separating the silica gel
- filtrationby filtration
- washthe silica gel was washed with chloroform
- distillationthe solvent was distilled off
- customthe resulting residue was purified by reverse-phase preparative HPLC