HRID456148

反应详情

EQUATION

反应方程式

HRID 456148 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the 6-(1-ethoxyvinyl)-3-(1-(6-fluoro-1-methyl-1H-indazol-5-yl)ethyl)-imidazo[1,2-b]pyridazine (450 mg, 0.985 mmol) in acetic acid (8 mL), was added 3N HCl (0.5 mL). The solution was stirred at rt for 2 h and the solvents were removed under reduced pressure. The residue was diluted with water and its pH was adjusted to basic with aqueous NaHCO3, extracted with DCM. The organic layer was washed with NaHCO3(aq) and brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by silica gel column chromatography to give yellow solid 1-(3-(1-(6-fluoro-1-methyl-1H-indazol-5-yl)ethyl)imidazo[1,2-b]pyridazin-6-yl)ethanone (300 mg, 81%). LCMS (method B): [MH]+=338, tR=2.49 min.

WORKUP

后处理

  1. customthe solvents were removed under reduced pressure
  2. additionThe residue was diluted with water and its pH
  3. extractionextracted with DCM
  4. washThe organic layer was washed with NaHCO3(aq) and brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by silica gel column chromatography