Hydrochloric Acid → Dimethyl {2-oxo-3-[3-(trifluoromethyl)phenoxy]propyl}phosphonate
反応式
[F:1][C:2]([F:25])([F:24])[C:3]1[CH:4]=[C:5]([CH:21]=[CH:22][CH:23]=1)[O:6][CH2:7][C:8](=NNC(N)=O)[CH2:9][P:10](=[O:15])([O:13][CH3:14])[O:11][CH3:12].C(Cl)Cl.Cl.[OH2:30]>>[F:1][C:2]([F:25])([F:24])[C:3]1[CH:4]=[C:5]([CH:21]=[CH:22][CH:23]=1)[O:6][CH2:7][C:8](=[O:30])[CH2:9][P:10](=[O:15])([O:13][CH3:14])[O:11][CH3:12]参加物
5
実験手順
A mixture of dimethyl 3-[3-(trifluoromethyl)phenoxy]-2-semicarbazonopropylphosphonate (19.2 g, 50 mmol), CH2Cl2 (50 mL) and 6 N HCl (50 mL) was stirred for 2 h at rt. Water (50 mL) was added to the mixture. The organic layer was separated, washed with brine, dried over Na2SO4, filtered through short column of silica gel and concentrated in vacuo to give 15.1 g (93%) of dimethyl 3-[3-(trifluoromethyl)phenoxy]-2-oxopropylphosphonate as light yellow oil. 1H NMR (CDCl3) δ: 7.42 (t, J=8.0 Hz, 1H), 7.22 (d, J=8.0 Hz, 1H), 7.11 (s, 1H), 7.07 (d, J=8.0 Hz, 1H), 4.77 (s, 2H), 3.80 (s, 3H), 3.74 (s, 3H), 3.23 (d, J=12 Hz, 2H).