反应详情

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).

1. customThe organic layer was separated
2. washwashed with brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered through short column of silica gel
5. concentrationconcentrated in vacuo