反应详情

The title compound was prepared according to the procedure for diethyl (4-{[4-chloro-5-(trifluoromethyl)pyrimidin-2-yl]amino}benzyl)phosphonate using ethyl(4-aminobenzyl)methylphosphinate (Compound 174B, 1.08 g, 5.07 mmol) and 2,4-dichloro-5-trifluoromethylpyrimidine. (1.0 g, 4.6 mmol). The compound was purified on an Isco Combiflash eluting with 0 to 10% MeOH in EtOAc. The compound was re-crystallized in EtOAc (˜20 mL) to afford 1.1 g, 61% yield, of the title compound. 1H NMR (400 MHz, DMSO-d6) δ 10.64 (s, 1H), 8.79 (d, J=0.51 Hz, 1H), 7.62 (d, J=8.34 Hz, 2H), 7.25 (dd, J=2.27, 8.59 Hz, 2H), 3.86-4.01 (m, 2H), 3.15 (d, J=17.68 Hz, 2H), 1.31 (d, J=13.64 Hz, 3H), 1.19 (t, J=6.95 Hz, 3H); MS (ES+): m/z: 396.0708 [MH+]. HPLC: tR=1.41 min (UPLC TOF MS: polar—3 min).

1. customThe compound was purified on an Isco Combiflash
2. washeluting with 0 to 10% MeOH in EtOAc
3. customThe compound was re-crystallized in EtOAc (˜20 mL)
4. customto afford 1.1 g, 61% yield
5. customHPLC: tR=1.41 min (UPLC TOF MS: polar—3 min)