反应详情

A mixture of Example 61a (1.70 g, 6.44 mmol) and 2,2-dimethylpropane-1,3-diamine (10 mL) was heated in a Biotage microwave reactor at 160° C. for 25 minutes. The solution was diluted with 20% brine and washed with EtOAc (2×). The combined organic layers were washed with 20% brine, dried (MgSO4), filtered, and concentrated. The residue was triturated with EtOAc and diethyl ether. The solids were filtered, washed with ether, and dried to give 1.19 g of the title compound. 1H NMR (300 MHz, DMSO-d6) ppm 0.87 (s, 6H), 2.36 (s, 2H), 3.16 (d, J=6.10 Hz, 2H), 6.78-6.89 (m, 2H), 6.97 (d, J=1.02 Hz, 1H), 7.21 (dd, J=7.97, 4.58 Hz, 1H), 8.13 (s, 1H), 8.27-8.38 (m, 2H). MS (ESI+) m/z 329.9 (M+H)+.

1. washwashed with EtOAc (2×)
2. washThe combined organic layers were washed with 20% brine
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was triturated with EtOAc and diethyl ether
7. filtrationThe solids were filtered
8. washwashed with ether
9. customdried