Ethyl 3-(2-amino-3,5-bis(trifluoromethyl)phenylamino)-3-oxopropanoate → ethyl 2-(5,7-bis(trifluoromethyl)-1H-benzo[d]imidazol-2-yl)acetate
反応式
[NH2:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][C:5]([C:12]([F:15])([F:14])[F:13])=[CH:4][C:3]=1[NH:16][C:17](=O)[CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20]>C(O)(=O)C.C1COCC1>[F:15][C:12]([F:13])([F:14])[C:5]1[CH:6]=[C:7]([C:8]([F:11])([F:10])[F:9])[C:2]2[NH:1][C:17]([CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])=[N:16][C:3]=2[CH:4]=1参加物
3
実験手順
A solution of ethyl 3-(2-amino-3,5-bis(trifluoromethyl)phenylamino)-3-oxopropanoate (330 mg, 0.92 mmol) in 3:1 acetic acid/THF (4 mL) was heated at reflux for 18 h. The mixture was concentrated in-vacuo, and the residue was purified over silica gel, eluting with 20%-30%-40% EtOAc/heptane, to yield 256 mg of a colorless oil as product. 1H NMR (500 MHz, DMSO) δ ppm 1.20 (m, 3 H) 4.11 (m, 4 H) 7.82 (m, 1 H) 8.28 (m, 1 H) 13.37 (m, 1 H).