反应详情

2.2 g of ethyl (E)-3-[2-(2,2,2-trifluoroethylcarbamoyl)-5-trifluoromethylphenyl]acrylate (5.9 mmol) were dissolved in 10 ml of methanol and 1.5 ml of a 5 M aqueous NaOH solution (7.5 mmol) were added. The mixture was stirred at RT for 18 h and then set to pH=7 using aqueous HCl solution. The solvents were removed under reduced pressure and the residue was suspended in 10 ml of water. This suspension was set to pH=2 using a 2N aqueous HCl solution and extracted 3 times with 10 ml each time of EA. Drying was effected over Na2SO4 and the solvent was removed under reduced pressure. The residue was crystallized with diethyl ether/DIP, mp: 202-204° C.

1. customThe solvents were removed under reduced pressure
2. extractionextracted 3 times with 10 ml each time of EA
3. customDrying
4. customthe solvent was removed under reduced pressure
5. customThe residue was crystallized with diethyl ether/DIP, mp: 202-204° C.