HRID877073

反应详情

EQUATION

反应方程式

HRID 877073 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

206.7 mg Crude 5-[2-(4-{1-[(tert-butoxycarbonyl)amino]cyclobutyl}phenyl)-3-phenylpyrimido[1,2-b]indazol-8-yl]pyrazole-1-carboxylic acid tert-butyl ester, intermediate example Int-3-0, were dissolved in 15 mL 4 M hydrogen chloride in dioxane. The reaction mixture was stirred over night at room temperature. After evaporation of the solvent the residue was dissolved in methanol and given on a PoraPak Rxn CX column. The column was washed with 100 mL methanol, and the product was eluted with methanol/ammonia. The solvent was removed, and the residue was purified by HPLC yielding 32.8 mg of the title compound.

WORKUP

后处理

  1. customAfter evaporation of the solvent the residue
  2. dissolutionwas dissolved in methanol
  3. washThe column was washed with 100 mL methanol
  4. washthe product was eluted with methanol/ammonia
  5. customThe solvent was removed
  6. customthe residue was purified by HPLC