反应详情

Triethylamine (5.58 g, 0.055 mol) is added dropwise to a mixture of 4-(p-chlorophenyl)-2-(tri-fluoromethyl)-5(2H)-oxazolone (15.6 g, 0.054 mol), methyl α-chloroacrylate (6.52. g, 0.054 mol) and acetonitrile (50 mL). The reaction mixture heats up to 55° C. during the addition. After the addition is complete, the reaction mixture is heated at reflux temperature for one hour, cooled to room temperature and filtered. The filtrate is poured into an ether/water mixture and extracted with ether. The combined organic extracts are dried over anhydrous magnesium sulfate and concentrated in vacuo to give a black residue. Recrystallization of the residue from hexane gives the title compound as an orange solid (8.25 g, 50.2%). Indentified by NMR spectral analyses.

1. additionThe reaction mixture heats up to 55° C. during the addition
2. additionAfter the addition
3. temperaturethe reaction mixture is heated
4. temperatureat reflux temperature for one hour
5. filtrationfiltered
6. additionThe filtrate is poured into an ether/water mixture
7. extractionextracted with ether
8. dry with materialThe combined organic extracts are dried over anhydrous magnesium sulfate
9. concentrationconcentrated in vacuo
10. customto give a black residue
11. customRecrystallization of the residue from hexane