反应详情

2-(3-Methylbenzoyl)-3-phenyl acrylic acid ethyl ester (1 g, 3.39 mmol) obtained in Step 2 was dissolved in dichloromethane, and methanesulfonic acid (5.22 g, 54.35 mmol) was added thereto, followed by stirring for 3 hrs at RT. Once the reaction was completed, the mixture was cooled to 0° C., neutralized with sodium bicarbonate, and extracted with dichloromethane. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography to obtain 273 mg of the titled compound (yield: 27%).

1. temperaturethe mixture was cooled to 0° C.
2. extractionextracted with dichloromethane
3. customThe organic layer was separated
4. dry with materialdried over anhydrous MgSO4
5. concentrationconcentrated under a reduced pressure
6. customThe resulting residue was purified by flash chromatography