反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
0.6 g. of 3',4'-anhydro-vinblastine are dissolved in 75 ml. of dimethyl formamide. Oxygen is bubbled through the solution slowly for 10 minutes, whereupon the reaction mixture is allowed to stand at room temperature for 16 to 20 hours. The pH is adjusted to 8.5 with a concentrated aqueous ammonium hydroxide solution. The alkaline mixture obtained is extracted with three 100-ml. portions of benzene. The combined extracts are dried with sodium sulphate, filtered and the filtrate is evaporated. The residue is dissolved in 3 ml. of ethanol and allowed to stand at 5° C. for 16 hours. The precipitated crystals are filtered off, washed with a small portion of cool methanol and dried. 0.366 mg. (61.0%) of the named compound is obtained.
WORKUP
后处理
- customOxygen is bubbled through the solution slowly for 10 minutes, whereupon the reaction mixture
- customThe alkaline mixture obtained
- extractionis extracted with three 100-ml
- dry with materialThe combined extracts are dried with sodium sulphate
- filtrationfiltered
- customthe filtrate is evaporated
- dissolutionThe residue is dissolved in 3 ml
- waitto stand at 5° C. for 16 hours
- filtrationThe precipitated crystals are filtered off
- washwashed with a small portion of cool methanol
- customdried