HRID2042841

反应详情

EQUATION

反应方程式

HRID 2042841 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of N-{2,4-dichloro-3-[6-(trans-4-trifluoromethyl-cyclohexylcarbamoyl)-5-(2,2-difluoro-ethoxy)-3H-imidazo[4,5-b]pyridin-2-ylamino]benzyl}-carbamic acid tert-butyl ester (6.3 g, 9.3 mmol), 4 M HCl in dioxane (60 ml) and MeOH (5 ml) is stirred for 15 min. The mixture is concentrated, diluted with water and basified with conc. NH3. The precipitate is collected by filtration, washed with water, dried and purified via prep HPLC. The product fractions are concentrated, basified with conc. NH3, extracted with EtOAc. The organic phases are dried with Na2SO4 and concentrated to give the crude sub-title compound (4.8 g).

WORKUP

后处理

  1. concentrationThe mixture is concentrated
  2. additiondiluted with water and basified with conc. NH3
  3. filtrationThe precipitate is collected by filtration
  4. washwashed with water
  5. customdried
  6. custompurified via prep HPLC
  7. concentrationThe product fractions are concentrated
  8. extractionextracted with EtOAc
  9. dry with materialThe organic phases are dried with Na2SO4
  10. concentrationconcentrated