反应详情

A stirred mixture of 26.05 g of 1,8-diaminonaphthalene, 32.66 g of 2-tridecanone, 55 mg of p-toluenesulfonic acid monohydrate, and 250 mL of toluene was heated to reflux under a nitrogen atmosphere using a Dean-Stark trap to remove the water evolved from the reaction for 5 hr. The mixture was then washed with saturated sodium bicarbonate solution, dried over anhydrous potassium carbonate, filtered, and the solvent removed under reduced pressure. The product was distilled to yield 48.86 g of dihydroperimidine intermediate, bp 192°-213° C. at 0.3 to 0.4 torr.

1. temperaturewas heated
2. temperatureto reflux under a nitrogen atmosphere
3. customto remove the water
4. customevolved from the reaction for 5 hr
5. washThe mixture was then washed with saturated sodium bicarbonate solution
6. dry with materialdried over anhydrous potassium carbonate
7. filtrationfiltered
8. customthe solvent removed under reduced pressure
9. distillationThe product was distilled