반응 #640610
ord-7efd57db705e42b4904f203238bd83f2
반응 방정식
반응 조건
후처리
- 1기타The organic layer was separated
- 2추출aqueous solution was extracted with dichloromethane (2×20 mL)
- 3건조The combined organic layer and extracts were dried over sodium sulfate
- 4기타evaporated to dryness
실험 절차
Vinblastine sulfate was purchased from Asian Talent. A 610-mg sample of vinblastine sulfate was dissolved in 20 mL of dichloromethane and then it was shaken with 20 mL of 5% aqueous sodium carbonate. The organic layer was separated and aqueous solution was extracted with dichloromethane (2×20 mL) and then with chloroform (20 mL). The combined organic layer and extracts were dried over sodium sulfate and evaporated to dryness, affording 526 mg (97%) of vinblastine free base as a sticky white solid. The purity of vinblastine free base was checked by 1H 300 MHz NMR and HPLC (99.1% AUC) using a Varian CHROMSEP HPLC column SS 250×4.6 mm including holder with guard column, MICROSORB 100-5 C18; gradient: 30/70 (0.1% trifluoroacetic acid in acetonitrile)/(0.1% trifluoroacetic acid in water) to 100/0 (0.1% trifluoroacetic acid in acetonitrile)/(0.1% trifluoroacetic acid in water); detection at 254 nm and 270 nm.