Reaktion #2441729

Reaktionsgleichung

compound 14

9-Methyl-2,3,4,7,8,9,10,11-octahydro-[1]benzothieno[2′,3′:4,5]pyrimido[1,2-a]azepin-13(1H)-one

potassium peroxodisulfate

→

2,3,8,9,10,11-Hexahydro-9-methyl-[1]benzothieno[2′,3′: 4,5]pyrimido[1,2-a]azepine-4,13(1H,7H)-dione

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture was heated
2. 2
   Temperaturto reflux for 30 minutes
3. 3
   SonstigeThe reaction was quenched with water
4. 4
   Extraktionextracted with CH2Cl2
5. 5
   WaschenThe organic layer was washed with 10% sodium thiosulfate and brine
6. 6
   Trocknendried over Na2SO4
7. 7
   FiltrationAfter filtration the solvent w
8. 8
   Sonstigeas evaporated
9. 9
   Sonstigethe product purified by flash chromatography

Vorschrift

To compound 14 (4.0 g, 13.9 mmol), potassium peroxodisulfate (11.3 g, 41.6 mmol) and CuSO4.5H2O, 250 ml of acetinitrile/water 1:1 were added. The reaction mixture was heated to reflux for 30 minutes. The reaction was quenched with water and extracted with CH2Cl2. The organic layer was washed with 10% sodium thiosulfate and brine, and dried over Na2SO4. After filtration the solvent w as evaporated and the product purified by flash chromatography using CH2Cl2/EtOAc 9:1 as an eluent.

Quelle