反应详情

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

1. additionThe reaction mixture was poured onto ice
2. extractionextracted three times with ethyl acetate
3. dry with materialdried the organic extracts over magnesium sulfate
4. filtrationfiltered
5. customevaporated to a yellow solid
6. customThe yellow solid (crude material) was purified
7. washeluting with 30% ethyl acetate/hexane