Reaktion #4563

Reaktionsgleichung

methylether

TPC-A

methyl iodide

→

methylether of TPC-A

Lösungsmittel

1,2-dimethoxy ethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter completion of the reaction
2. 2
   Filtrationthe solution was filtered
3. 3
   workup.DISTILLATIONthe filtrate was subjected to distillation in vacuo
4. 4
   Sonstigeto remove solvent
5. 5
   Sonstigethe residue obtained
6. 6
   Sonstigewas purified by P-TLC
7. 7
   Sonstigefollowed by the recrystallization from methanol

Vorschrift

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).

Quelle