反应详情

The dehydration of 5-hydroxy-5-trifluoromethyl-3,4,5,8-tetrahydro-2H,6H-1-thia-4,8-diaza-phenanthren-7-one (69 mg, 0.23 mmol) was carried out in concentrated sulfuric acid at 150° C. The solution was cooled to about rrom temperature, added to ice water, made basic with 1M sodium carbonate, extract with ethyl acetate three times, the organic layers washed with brine, dried over sodium sulfate, filtered and the filtrate evaporated to yield 5-trifluoromethyl-3,4-dihydro-2H,8H-1-thia-4,8-diaza-phenanthren-7-one as a green solid.

1. temperatureThe solution was cooled to about rrom temperature
2. extractionextract with ethyl acetate three times
3. washthe organic layers washed with brine
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. customthe filtrate evaporated