HRID69295

反应详情

EQUATION

反应方程式

HRID 69295 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvent was removed
  2. customThe residue was purified by preparative HPLC with acetonitrile and water (+0.1% TFA)
  3. customthe acetonitrile was removed
  4. extractionwas extracted with EtOAc twice
  5. washCombined organic layers was washed with brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated