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
720 mg (1.3 mmol) Crude {1-[4-(9-fluoro-4-cyclopropylamino-3-phenyl-pyrimido[1,2-b]indazol-2-yl)phenyl]cyclobutyl}carbamic acid tert-butyl ester, described in step 2, were dissolved in 36 mL dioxane. After dropwise addition of 36 mL of a 4 M hydrogen chloride in dioxane the reaction mixture was stirred for five hours at room temperature. The reaction mixture was evaporated to dryness. Saturated aqueous sodium bicarbonate solution was added and the reaction mixture was extracted three times with ethyl acetate. The combined organic extracts were washed with brine and dried. After evaporation of the solvent the residue was purified by HPLC to yield 44.3 mg of the desired compound which was 90% pure.
WORKUP
后处理
- customThe reaction mixture was evaporated to dryness
- additionSaturated aqueous sodium bicarbonate solution was added
- extractionthe reaction mixture was extracted three times with ethyl acetate
- washThe combined organic extracts were washed with brine
- customdried
- customAfter evaporation of the solvent the residue
- customwas purified by HPLC