반응 #155664

반응 방정식

acetic anhydride

Endothall

→

product

수율 50.6%

Endothall Anhydride

수율 50.6%

용매

benzene

반응 조건

후처리

1. 1
   기타had gone into solution (2 hours)
2. 2
   온도The solution was heated under vacuum
3. 3
   기타to remove the benzene
4. 4
   workup.ADDITIONPetroleum ether (5 mL) was then added
5. 5
   기타the desired anhydride spontaneously crystallized
6. 6
   기타The product was removed by filtration
7. 7
   세척washed with a little petroleum ether

실험 절차

As shown in scheme 1, we prepared endothal anhydride by adding acetic anhydride (0.5 mL) (4) to a suspension of Endothall (186 mg) (3) in benzene (3 mL) and the mixture was then stirred until the solid had gone into solution (2 hours). The solution was heated under vacuum to remove the benzene and the residue was then heated at 80° C. for 30 min. Petroleum ether (5 mL) was then added and the desired anhydride spontaneously crystallized. The product was removed by filtration washed with a little petroleum ether to give the pure product (85 mg) which was used immediately in the following two preparations.

출처