反应详情

A suspension of diethyl (4-{[4-({7-[1-(3-hydroxypropyl)-1H-pyrazol-4-yl]-2-methyl-3-oxo-2,3-dihydro-1H-isoindol-4-yl}amino)-5-(trifluoromethyl)pyrimidin-2-yl]amino}-3-methoxybenzyl)phosphonate (Compound 1B, 255 mg, 0.36 mmol) and sodium iodide (606 mg, 4.04 mmol) in 2-butanone (5 mL) was subjected to 7 hours of microwave irradiation at 120° C. A solid precipitated, which filtered off, rinsed several times with ice cold acetone, and dried thoroughly to afford the desired compound as 277 mg as a light yellow solid. 1H NMR (400 MHz, DMSO-d6) δ 10.64 (s, 1H), 9.26 (br s, 1H), 9.08 (s, 1H), 8.34 (s, 1H), 8.15 (br s, 2H), 7.71 (s, 1H), 7.13 (d, J=7.6 Hz, 1H), 7.08 (s, 1H), 6.89 (d, J=7.8 Hz, 1H), 6.45 (br s, 1H), 4.60 (s, 2H), 4.19 (t, J=6.1 Hz, 2H), 3.68 (s, 3H), 3.60-3.67 (m, 2H), 3.45 (q, J=5.9 Hz, 2H), 3.09 (s, 3H), 2.77 (d, J=19.7 Hz, 2H), 1.94 (quin, J=5.9 Hz, 2H), 0.94 (t, J=7.1 Hz, 3H). MS (ESI): m/z 676.30 [M+H]+. UPLC: tR=1.06 min (UPLC-SQD: analytical—2 min).

1. customwas subjected to 7 hours of microwave irradiation at 120° C
2. customA solid precipitated
3. filtrationwhich filtered off
4. washrinsed several times with ice cold acetone
5. customdried thoroughly