반응 #1856080

반응 방정식

1,8-diaminonaphthalene

2-tridecanone

→

dihydroperimidine

수율 174.3%

용매

toluene

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도to reflux under a nitrogen atmosphere
3. 3
   기타to remove the water
4. 4
   기타evolved from the reaction for 5 hr
5. 5
   세척The mixture was then washed with saturated sodium bicarbonate solution
6. 6
   건조dried over anhydrous potassium carbonate
7. 7
   여과filtered
8. 8
   기타the solvent removed under reduced pressure
9. 9
   workup.DISTILLATIONThe product was distilled

실험 절차

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.

출처