Ethanol → HCID 58841918、化合物
反応式
[F:1][C:2]([F:13])([F:12])[C:3](=O)[CH2:4][C:5](=O)[C:6]([F:9])([F:8])[F:7].Cl.[NH:15]([C:17]1[CH:25]=[CH:24][C:20]([C:21]([OH:23])=[O:22])=[CH:19][CH:18]=1)[NH2:16].[CH2:26](O)[CH3:27]>>[CH2:26]([O:22][C:21](=[O:23])[C:20]1[CH:19]=[CH:18][C:17]([N:15]2[C:3]([C:2]([F:13])([F:12])[F:1])=[CH:4][C:5]([C:6]([F:9])([F:8])[F:7])=[N:16]2)=[CH:25][CH:24]=1)[CH3:27]参加物
4
反応条件
- 温度
- 100 °C
実験手順
A mixture of 1,1,1,5,5,5-hexafluoro-pentane-2,4-dione (3.16 g, 15.2 mmol) and 4-hydrazinobenzoic acid hydrochloride (2.86 g, 15.2 mmol) in ethanol (5 mL) was stirred at 100° C. in a sealed tube for 4 hours. The mixture was cooled to room temperature and the solvent was removed under reduced pressure. The residue was purified by chromatography (SiO2, 4:1 to 3:1 hexane/EtOAc) to give 4-(3,5-bis-trifluoromethyl-pyrazol-1-yl)-benzoic acid ethyl ester, (3.1 g, 58% yield) as a syrup: 1H-NMR (CDCl3) δ 1.40 (t, 3H, J=7), 4.35–4.50 (m, 2H), 7.10 (s, 1H), 7.60 (d, 2H, J=7), 8.21 (d, 2H, J=7) ppm.