反应详情

4-Amino-2-(1-methyl-1H-pyrazol-5-yl)phenol (300.00 mg, 1585.5 μmol), methanesulfonic acid 2-(S)-tert-butoxycarbonylamino-propyl ester (602.45 mg, 2378.3 μmol) and Cesium carbonate (1033.2 mg, 3171.0 μmol) were dissolved in acetone, and heated in the microwave at 130 C for 1 hour. The reaction mixture was filtered and the filtrate removed under vacuum. The residue was dissolved in DCM; washed with 1N NaOH (3×) and then removed under vacuum to yield a brownish residue in 34.6% yield. LCMS m/z=347.3 (M+H); 1H NMR (400 MHz, DMSO-d6) δ ppm 1.16 (d, J=6.32 Hz, 3H), 1.38 (s, 9H), 3.65 (s, 3H), 3.67-3.77 (m, 3H), 6.23 (d, J=1.77 Hz, 1H), 6.84 (s, 1H), 6.95 (s, 1H), 7.11 (s, 1H), 7.44 (d, J=1.77 Hz, 1H).

1. temperatureheated in the microwave at 130 C for 1 hour
2. filtrationThe reaction mixture was filtered
3. customthe filtrate removed under vacuum
4. dissolutionThe residue was dissolved in DCM
5. washwashed with 1N NaOH (3×)
6. customremoved under vacuum
7. customto yield a brownish residue in 34.6% yield