反应详情

温度

60 °C

A suspension of 4-[1-(1-methyl-2-{4-[(1-methyl-1H-pyrazol-3-yl)sulfonyl]piperazin-1-yl}ethyl)-1H-pyrazol-4-yl]-7H-pyrrolo[2,3-d]pyrimidine (0.165 g, 0.362 mmol) in isopropyl alcohol (60 mL) was heated at 60° C. until becoming clear. Phosphoric acid (0.0373 g, 0.373 mmol) in isopropyl alcohol (1.0 mL) was added to the solution at 60° C. The solution was cooled down but no precipitation formed. Solvents were reduced in vacuo until white solid precipitated and held at RT for 30 min. The solid was filtered off, air dried, rinsed with some Et2O and again air dried to give a phosphoric acid salt (150 mg, 74.8%). The number of phosphoric acids in the salt was not determined. LCMS calculated for C20H26N9O2S(M+H)+: m/z=456.2 (free base); Found: 456.4. 1H NMR (400 MHz, DMSO-d6): δ 8.62 (1H, s), 8.59 (1H, s), 8.22 (1H, s), 7.86 (1H, d, J=2.2 Hz), 7.54 (1H, d, J=3.6 Hz), 6.91 (1H, d, J=3.6 Hz), 6.58 (1H, d, J=2.2 Hz), 4.63 (1H, m), 3.82 (3H, s), 2.85˜2.78 (5H, m), 2.61˜2.54 (3H, m), 2.36 (2H, m), 1.40 (3H, d, J=6.4 Hz) ppm.

1. temperatureThe solution was cooled down
2. customno precipitation
3. customformed
4. customprecipitated
5. filtrationThe solid was filtered off
6. customair dried
7. washrinsed with some Et2O and again air
8. customdried