反应详情

150 g of 2-(4-chloro-4,4-difluoro-but-1-yl)malonic acid diethyl ester, 160 g of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) and 250 ml of toluene are stirred for 15 hours at reflux temperature. After cooling, 200 ml of toluene are added and the reaction mixture is washed with 500 ml of water and then with 500 ml of 2N NaCl solution, dried over sodium sulfate and the solvent is evaporated off. The residue is distilled at 65° and 0.052 mbar. The title product is obtained in the form of a colourless oil.

1. temperatureat reflux temperature
2. temperatureAfter cooling
3. washthe reaction mixture is washed with 500 ml of water
4. dry with materialwith 500 ml of 2N NaCl solution, dried over sodium sulfate
5. customthe solvent is evaporated off
6. distillationThe residue is distilled at 65°