反应详情

To a solution of 2,4-Dichloro-5-trifluoromethyl-pyrimidine (963 mg, 4.43 mmol) in 30 mL of 50/50 mixture of t-BuOH/DCE was added a solution of ZnCl2 (1M in THF;4.43 mL). After one hour 6-Amino-3,4-dihydro-1H-quinolin-2-one (480 mg;2.95 mmol) was added followed by the dropwise addition of triethylamine (0.617 ml, 4.43 mmol) in 2 mL t-BUOH/DCE. Following removal of the solvent under reduced pressure, the crude reaction was triturated from methanol and the product filtered off as a yellow solid 723 mg (72% yield). 1H NMR (DMSO-d6, 400 MHz) δ 2.39 (t, J=12 Hz; 2H), 2.80 (t, J=8 Hz; 2H), 6.78 (d, J=8 Hz; 1H), 7.35 (d, J=8 Hz; 1H), 7.40 (br s, 1H), 8.70 (s, 1H), 10.02 (s, 1H), 10.48 (s, 1H). HPLC ret. time: 6.074 (96% purity), LRMS (M+) 343.2/345.2.

1. customremoval of the solvent under reduced pressure
2. customthe crude reaction
3. customwas triturated from methanol