反应详情

A mixture of sodium acetate (0.56 g), 2,4,6-trichloroquinazoline (0.40 g) and 4'-aminomethyl (1,1'-biphenyl)-2-carboxylic acid (0.43 g) was stirred at room temperature in 10 mL of THF for 5 days. All solvents were removed by evaporation and the resulting residue was partitioned between ethyl acetate and brine. The ethyl acetate fraction was dried over anhydrous magnesium sulfate, filtered and evaporated. The crude material was purified using silica gel chromatography to yield 0.15 g (21%) of an off white solid (m.p.=210°-240° C.): 1H NMR (DMSO-d6, 400 MHz) δ9.45 (t, J=6.2 Hz, 1H), 8.52 (d, J=2.3 Hz, 1H), 7.83 (dd, J=2.3, 8.9 Hz, 1H), 7.66 (m, 2H), 7.49 (m, 1H), 7.35 (m, 7H), 4.77 (d, J=5.2 Hz); negative FAB MS m/e 422(M-H). Anal. calcd for C22H15Cl2N3O2 : C, 62.28; H,3.56; N, 9.90. Found: C, 62.44; H, 3.52; N, 9.95.

1. customAll solvents were removed by evaporation
2. customthe resulting residue was partitioned between ethyl acetate and brine
3. dry with materialThe ethyl acetate fraction was dried over anhydrous magnesium sulfate
4. filtrationfiltered
5. customevaporated
6. customThe crude material was purified