Formamidine acetate → HCID 57758181, 화합물
반응식
C(O)(=O)C.[CH:5](N)=[NH:6].[NH2:8][N:9]1[C:13]([C:14]#[N:15])=[C:12]([C:16]2[CH:21]=[CH:20][C:19]([NH2:22])=[C:18]([F:23])[CH:17]=2)[C:11]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[CH:10]1>C(O)CCC>[NH2:15][C:14]1[C:13]2=[C:12]([C:16]3[CH:21]=[CH:20][C:19]([NH2:22])=[C:18]([F:23])[CH:17]=3)[C:11]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[CH:10][N:9]2[N:8]=[CH:5][N:6]=1참가 물질
4
반응 조건
- 온도
- 100 °C
실험 절차
Formamidine acetate (22.4 g, 215 mmol) was added to a suspension of ethyl 1-amino-4-(4-amino-3-fluorophenyl)-5-cyano-1H-pyrrole-3-carboxylate (6.2 g, 21.5 mmol) in n-butanol (100 mL). The reaction was heated (100° C.) for 16 h and then cooled to rt. The solvent was removed under reduced pressure and then ethanol (50 mL) and water (200 mL) were added. The mixture was stirred for 30 min and the resulting precipitate was collected by filtration. The solid was washed with water (2×50 mL) and dried to afford desired product (5.80 g, 85%); 1H NMR (300 MHz, DMSO-d6) δ 8.08 (s, 1H), 8.00-8.10 (br s, 1H), 7.90 (s, 1H), 7.03 (dd, J=12.3, 1.9 Hz, 1H), 6.77-6.88 (m, 2H), 5.36 (s, 2H), 5.21-5.31 (br s, 1H), 4.06 (q, J=7.1 Hz, 2H), 1.11 (t, J=7.1 Hz, 3H); ES-MS m/z 316.4 (MH)+; HPLC RT (Method B) 2.39 min.