HRID2049976

反应详情

EQUATION

反应方程式

HRID 2049976 的结构方程式

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

  1. customOxygen is bubbled through the solution slowly for 10 minutes, whereupon the reaction mixture
  2. customThe alkaline mixture obtained
  3. extractionis extracted with three 100-ml
  4. dry with materialThe combined extracts are dried with sodium sulphate
  5. filtrationfiltered
  6. customthe filtrate is evaporated
  7. dissolutionThe residue is dissolved in 3 ml
  8. waitto stand at 5° C. for 16 hours
  9. filtrationThe precipitated crystals are filtered off
  10. washwashed with a small portion of cool methanol
  11. customdried