反应详情

A suspension of 2.46 g of 3-aminopropylphosphonous acid in 20 ml of hexamethyldisilazane is heated to reflux under an inert gas for 24 hours. The resulting clear solution is cooled to 15° and 2.0 ml of cyclobutanone are added. An exothermic reaction ensues. The reaction mixture is stirred until the temperature drops to room temperature (approximately 1 hour). Water is added and the volatile materials are removed in vacuo to yield a semi-solid. This is dissolved in 2.0M aqueous hydrochloride acid and washed with 2×100 ml of dichloromethane. The aqueous layer is evaporated in vacuo to afford a solid which is passed through a DOWEX® 50 W×8 (14-40 mesh) ion-exchange column to give 3-aminopropyl(1-hydroxycyclobutyl)phosphinic acid, m.p. 174°-175° (dec).

1. temperatureis heated
2. temperatureto reflux under an inert gas for 24 hours
3. temperatureThe resulting clear solution is cooled to 15°
4. customAn exothermic reaction
5. customdrops to room temperature
6. custom(approximately 1 hour)
7. customthe volatile materials are removed in vacuo
8. customto yield a semi-solid
9. washwashed with 2×100 ml of dichloromethane
10. customThe aqueous layer is evaporated in vacuo
11. customto afford a solid which