反应详情

The crude 4-(3-aminocyclobutyl)-9-[1-(4-amino-3-methyl-1H-pyrazolo[3,4-d]pyrimidin-1-yl)ethyl]-7-chloro-2-methyl-2,3,4,5-tetrahydro-1,4-benzoxazepine-6-carbonitrile trishydrochloride was dissolved in N,N-dimethylformamide (2 mL) and triethylamine (10 μL, 0.1 mmol). To this mixture was added acetic anhydride (7.7 mg, 0.075 mmol). The reaction was stirred for 1 h at room temperature, and the reaction was purified without workup by prep HPLC on C-18 column eluting water:acetonitrile gradient buffered pH 10 to give two diastereomers: Peak #1 (Example 67): LCMS calculated for C25H30ClN8O2 (M+H)+: m/z=509.2; found: 509.2; Peak #2 (Example 68): LCMS calculated for C25H30ClN8O2 (M+H)+: m/z=509.2; found: 509.2.

1. customthe reaction was purified without workup by prep HPLC on C-18 column
2. washeluting water
3. customacetonitrile gradient buffered pH 10 to give two diastereomers