反应详情

In 10 ml of anhydrous dioxane was dissolved 1.15 g of ethyl 3-[(1R,2S)-2-fluorocyclopropylamino]-2-(2,3,4,5-tetrafluoro-6-methylbenzoyl)acrylate, and 190 mg of 60% sodium hydride in oil was added thereto, followed by stirring at room temperature for 30 minutes. The dioxane was concentrated to about half the volume, and the concentrate was added to 25 ml of 1N hydrochloric acid under cooling with ice. The crystals precipitated were collected by filtration, washed with diethyl ether, and dried to yield 1.05 g of the titled compound as a yellow crystal.

1. additionwas added
2. concentrationThe dioxane was concentrated to about half the volume
3. additionthe concentrate was added to 25 ml of 1N hydrochloric acid
4. temperatureunder cooling with ice
5. customThe crystals precipitated
6. filtrationwere collected by filtration
7. washwashed with diethyl ether
8. customdried