HRID4467

反应详情

EQUATION

反应方程式

HRID 4467 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 10 ml of anhydrous 1,2-dimethoxy ethane, 100 mg of the methylether derivative of TPC-A was dissolved and 240 mg of potassium fluoride-alumina and excess amount of methyl iodide were added and the mixture was shielded from the light while stirring at room temperature overnight. After completion of the reaction, the solution was filtered, the filtrate was subjected to distillation in vacuo to remove solvent and the residue obtained was purified by P-TLC followed by the recrystallization from methanol to obtain N-methyl derivative of the methylether of TPC-A (98 mg) as colorless crystal having m.p. of 285° to 292° C. (decomp) and [α]D27 of -166° (CHCl3).

WORKUP

后处理

  1. customAfter completion of the reaction
  2. filtrationthe solution was filtered
  3. distillationthe filtrate was subjected to distillation in vacuo
  4. customto remove solvent
  5. customthe residue obtained
  6. customwas purified by P-TLC
  7. customfollowed by the recrystallization from methanol