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 2,4-dichloro-5-trifluoromethylpyrimidine and diethyl[(5-amino-6-methoxypyridin-2-yl)methyl]phosphonate (Compound 286B). The crude material was purified by column chromatography (methylene chloride:CH3CN=0-20%) to obtain a mixture of 2 regioisomers with a ratio of roughly 4:1 (the major one is the desired title compound [364 mg, 61% yield]). 1H NMR (400 MHz, DMSO-d6) δ=1.22 (t, J=6.9 Hz, 6H), 3.35 (d, J=21.7 Hz, 2H), 3.87 (s, 3H), 4.00-4.07 (m, 4H), 6.98 (dd, J=7.8, 2.8 Hz, 1H), 7.83 (d, J=7.6 Hz, 1H), 8.72 (s, 1H), 9.90 (s, 1H). MS (ES+): m/z 455.21 (100), 457.15 (33) [MH+]; HPLC: tR=1.41 min (UPLC, Analytical).

1. customThe title compound was prepared
2. customThe crude material was purified by column chromatography (methylene chloride:CH3CN=0-20%)
3. customto obtain
4. additiona mixture of 2 regioisomers with a ratio of roughly 4:1 (the major one