反应详情

A suspension consisting of 50.1 g (0.32 mol) of benzamidine hydrochloride, 133 g (0.96 mol) of potassium carbonate, and 250 mL of tetrahydrofuran was heated under reflux for one hour, and the foregoing toluene solution of 2-bromo-1′-propionaphthone was added dropwise over 50 minutes. After completion of addition, heated under reflux for 2 hours. Next, the reaction mixture was concentrated in vacuo, the resulting concentrate was diluted with 200 mL of toluene, and the solution was poured into 600 mL of water. The mixture was stirred to precipitate a solid. This solid was collected by filtration, successively washed with toluene and water, and then dried to obtain a crude crystal as a desired material. This crude crystal was recrystallized from DMF to obtain 48.1 g (yield: 52.9%) of a white powder.

1. temperaturewas heated
2. temperatureunder reflux for one hour
3. additionAfter completion of addition
4. temperatureheated
5. temperatureunder reflux for 2 hours
6. concentrationNext, the reaction mixture was concentrated in vacuo
7. concentrationthe resulting concentrate
8. additionwas diluted with 200 mL of toluene
9. additionthe solution was poured into 600 mL of water
10. customto precipitate a solid
11. filtrationThis solid was collected by filtration
12. washsuccessively washed with toluene and water
13. customdried