Reference of 25597-16-4, A common heterocyclic compound, 25597-16-4, name is Ethyl 4,4,4-trifluorocrotonate, molecular formula is C6H7F3O2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
[0832] A mixture of 10 g (72.5 mmol) of 2, 4-dihydroxybenzaldehyde, 15.3 mL (101. 4 mmol) of ethyl 4-triflouromethylcrotonate, and 20 g (145 mmol) of potassium carbonate in 25 ML of anhydrous DIMETHYLFORMMAMIDE was heated to 90C for three h. After cooling to room temperature, the reaction was added to 500 mL of ethyl acetate. The organic phase was washed with brine three times, dried over anhydrous magnesium sulfate and CONCD in vacuo. Silica chromatography with EtOAc/hexane (3: 7) gave 19.0 g (98%) of a yellow solid: 1H NMR (CDC13/400 MHz) 7.63 (s, 1H), 6.85 (d, J=8. 8 Hz, 1H), 6.79 (dd, J=8.8Hz, 2.8Hz, 1H), 6.70 (d, J=2. 8 Hz, 1H), 5.63 (q, J=6. 8 Hz, 1H), 4. 31 (m, 2H), 1.34 (t, J=7. 2 Hz, 3H). MS (ESI+) 289. 1 (M+1, 100).
The synthetic route of 25597-16-4 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; PHARMACIA CORPORATION; WO2004/87686; (2004); A2;; ; Patent; PHARMACIA CORPORATION; WO2004/87687; (2004); A1;,
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