Reaktion #440331

Reaktionsgleichung

hydrogen peroxide

4-(6,7-dimethoxy-4-quinazolinyl)-N-(3,4-methylenedioxybenzyl)-1-piperazinethiocarboxamide

sodium thiosulfate

hydrochloric acid

sodium hydroxide

→

desired compound

Ausbeute 20.0%

4-(6,7-Dimethoxy-4-quinazolinyl)-N-(3,4-methylenedioxybenzyl)-1-piperazinecarboxamide

Ausbeute 20.0%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwere added
2. 2
   workup.ADDITIONwas added to the reaction mixture for neutralization
3. 3
   ExtraktionThe resulting mixture was extracted with dichloromethane
4. 4
   Waschenthe organic layer was washed with water
5. 5
   Trocknendried over sodium sulfate
6. 6
   SonstigeAfter the solvent was evaporated
7. 7
   Sonstigethe residue was purified by silica gel chromatography

Vorschrift

In 10 ml of ethanol was suspended 152.7 mg (0.33 mmol) of 4-(6,7-dimethoxy-4-quinazolinyl)-N-(3,4-methylenedioxybenzyl)-1-piperazinethiocarboxamide obtained in Example 208, and 1 ml of a 10 N aqueous solution of sodium hydroxide and 1 ml of 30% aqueous hydrogen peroxide were added thereto, followed by overnight stirring. After addition of an aqueous solution of sodium thiosulfate, 4 N hydrochloric acid was added to the reaction mixture for neutralization. The resulting mixture was extracted with dichloromethane, and the organic layer was washed with water and dried over sodium sulfate. After the solvent was evaporated, the residue was purified by silica gel chromatography to give the desired compound as colorless crystals.

Quelle