反应详情

To a 50 ml-reaction vessel were put 10 ml of MeOH, 1.9 mg of 3',4'-anhydrovinblastine (AVLB), and 1 ml of a MeOH solution of FeCl3 (1.2M), and the mixture was stirred for 30 min. under cooling with ice, while air was bubbled. Following addition of 9 mg of NaBH4, the mixture was stirred for additional 30 min. Then, 2 ml of 25% aqueous ammonia and 20 ml of water were added to make the solution basic. The products were extracted 3 times with 30 ml each of ethyl acetate. The extracts were combined and evaporated to dryness under reduced pressure at 40° or less. The resulting sample was analyzed by HPLC under the same condition of AVLB as well as less than 1% yield of vinblastine (VLB) and leurosidine (LEU) were obtained.

1. customTo a 50 ml-reaction vessel
2. temperatureunder cooling with ice, while air
3. customwas bubbled
4. additionaddition of 9 mg of NaBH4
5. stirringthe mixture was stirred for additional 30 min
6. additionThen, 2 ml of 25% aqueous ammonia and 20 ml of water were added
7. extractionThe products were extracted 3 times with 30 ml each of ethyl acetate
8. customevaporated to dryness under reduced pressure at 40° or less