反应详情

温度

80 °C

Oxirane, 2,2-dimethyl-(5.5 μL, 0.066 mmol) was added to a mixture of 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 bishydrochloride (16 mg, 0.039 mmol) and triethylamine (10 μL, 0.09 mmol) in N,N-dimethylformamide (2 mL). The reaction was heated at 80° C. for 3 hrs and was allowed to cool to room temperature. 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 65): LCMS calculated for C23H29ClN7O2 (M+H)+: m/z=470.2; found: 470.2; Peak #2 (Example 66): LCMS calculated for C23H29ClN7O2 (M+H)+: m/z=470.2; found: 470.2.

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