Reaktion #53426

Reaktionsgleichung

7-amino-6-hydroxy-6-trifluoromethyl-2,3,5,6-tetrahydro-1-oxa-3a-aza-phenalen-4-one

sodium carbonate

→

7-amino-6-trifluoromethyl-2,3-dihydro-1-oxa-3a-aza-phenalen-4-one

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONThe reaction mixture was poured onto ice
2. 2
   Extraktionextracted three times with ethyl acetate
3. 3
   Trocknendried the organic extracts over magnesium sulfate
4. 4
   Filtrationfiltered
5. 5
   Sonstigeevaporated to a yellow solid
6. 6
   SonstigeThe yellow solid (crude material) was purified
7. 7
   Wascheneluting with 30% ethyl acetate/hexane

Vorschrift

Impure 7-amino-6-hydroxy-6-trifluoromethyl-2,3,5,6-tetrahydro-1-oxa-3a-aza-phenalen-4-one (0.2 g) was heated to 140° C. for 1.5 hours then stirred at room temperature overnight. The reaction mixture was poured onto ice, made basic with 1M sodium carbonate, extracted three times with ethyl acetate, dried the organic extracts over magnesium sulfate, filtered, evaporated to a yellow solid. The yellow solid (crude material) was purified using the Biotage 40S system eluting with 30% ethyl acetate/hexane to yield 7-amino-6-trifluoromethyl-2,3-dihydro-1-oxa-3a-aza-phenalen-4-one

Quelle