反応 #155664

反応方程式

acetic anhydride

Endothall

→

product

収率 50.6%

Endothall Anhydride

収率 50.6%

溶媒

benzene

反応条件

後処理

1. 1
   その他had gone into solution (2 hours)
2. 2
   温度The solution was heated under vacuum
3. 3
   その他to remove the benzene
4. 4
   workup.ADDITIONPetroleum ether (5 mL) was then added
5. 5
   その他the desired anhydride spontaneously crystallized
6. 6
   その他The product was removed by filtration
7. 7
   洗浄washed with a little petroleum ether

実験手順

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.

出典