反应详情

A solution of 1,1-dimethylethyl 4-[({[6-amino-5-chloro-2-(methyloxy)-3-pyridinyl]carbonyl}amino)methyl]-1-piperidinecarboxylate (step 1 in example 1, 6.20 g, 15.5 mmol) in 10% methanolic hydrochloric acid (130 ml) was stirred at room temperature for 7 h. The mixture was concentrated to ca. 30 ml. The residue was basified with 2 N aqueous sodium hydroxide (pH=10) and the aqueous layer was extracted with dichloromethane (80 ml×3). The combined organic layer was dried over magnesium sulfate and concentrated in vacuo. The residue was chromatographed on a column of aminopropyl silica gel eluting with methanol/dichloromethane (1:15) to give 3.94 g (85%) of the title compound as a white solid.

1. concentrationThe mixture was concentrated to ca. 30 ml
2. extractionthe aqueous layer was extracted with dichloromethane (80 ml×3)
3. dry with materialThe combined organic layer was dried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe residue was chromatographed on a column of aminopropyl silica gel eluting with methanol/dichloromethane (1:15)