2,4-Dichloro-5-(trifluoromethyl)pyrimidine → 4-chloro-N-[4-(dipropyl phosphoryl)phenyl]-5-(trifluoromethyl)pyrimidin-2-amine
반응식
C(OP(C[C:10]1[CH:15]=[CH:14][C:13]([NH:16][C:17]2[N:22]=[C:21]([Cl:23])[C:20]([C:24]([F:27])([F:26])[F:25])=[CH:19][N:18]=2)=[CH:12][CH:11]=1)(=O)OCC)C.ClC1N=C(Cl)C(C(F)(F)F)=CN=1.[CH2:40]([P:43](C1C=CC(N)=CC=1)([CH2:45][CH2:46][CH3:47])=[O:44])[CH2:41][CH3:42]>>[Cl:23][C:21]1[C:20]([C:24]([F:25])([F:26])[F:27])=[CH:19][N:18]=[C:17]([NH:16][C:13]2[CH:12]=[CH:11][C:10]([P:43]([CH2:45][CH2:46][CH3:47])([CH2:40][CH2:41][CH3:42])=[O:44])=[CH:15][CH:14]=2)[N:22]=1참가 물질
4
실험 절차
The title compound was prepared according to the procedure for diethyl(4-{[4-chloro-5-(trifluoromethyl)pyrimidin-2-yl]amino}benzyl)phosphonate using 2,4-Dichloro-5-trifluoromethylpyrimidine (101.6 mg, 0.4681 mmol) and 4-(dipropylphosphoryl)aniline (Compound 198B: 116 mg, 0.515 mmol). This was purified on an ISCO Combiflash unit (0-5% MeOH/DCM) to isolate 75 mg of the desired product as a white solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 0.90 (t, J=7.3 Hz, 6H), 1.30 (br. s., 2H), 1.46 (br. s., 2H), 1.76-2.00 (m, 4H), 7.69 (dd, J=10.1, 8.6 Hz, 2H), 7.84 (dd, J=8.7, 1.9 Hz, 2H), 8.87 (s, 1H), 10.89 (s, 1H). MS (ES+): m/z=406.04 (100) 408.01 (35) [MH+]. HPLC: tR=4.01 min (ZQ3, polar—5 min)