HRID69295
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
PROCEDURE
实验过程
3-Imidazo[1,2-a]pyridin-6-ylmethyl-6-(1-methyl-1H-pyrazol-4-yl)-imidazo[1,2-b]pyridazine (Example 10, 33.6 mg, 0102 mmol) was dissolved in DCM (1 mL) with N-chlorosuccinimide (15 mg, 0.112 mmol). The RM was stirred at rt for 22 h. The solvent was removed. The residue was purified by preparative HPLC with acetonitrile and water (+0.1% TFA). The fractions were joined and the acetonitrile was removed. The aqueous solution was basified with 5% NaHCO3 solution and it was extracted with EtOAc twice. Combined organic layers was washed with brine and dried over Na2SO4, filtered and concentrated to afford the white title compound (tR 0.7 min (conditions 2), MH+=364).
WORKUP
后处理
- customThe solvent was removed
- customThe residue was purified by preparative HPLC with acetonitrile and water (+0.1% TFA)
- customthe acetonitrile was removed
- extractionwas extracted with EtOAc twice
- washCombined organic layers was washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated