반응 #79376

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2-amino-4-fluoro-5-iodo-benzoic acid

trichloromethylchloroformate

→

title compound

수율 90.4%

4-Fluoro-5-iodo-isatoic anhydride

수율 90.4%

용매

—

hexanes

dioxane

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후처리

1. 1
   기타equipped with a magnetic stir bar
2. 2
   온도reflux condenser
3. 3
   온도heated
4. 4
   온도to reflux for 16 hours
5. 5
   온도to cool
6. 6
   여과The solid was collected by suction filtration
7. 7
   세척washed with an additional 0.5 liters of hexanes
8. 8
   기타dried under vacuum at room temperature

실험 절차

Anhydrous dioxane (0.5 liters), 2-amino-4-fluoro-5-iodo-benzoic acid (46 grams, 164 mmoles), and trichloromethylchloroformate (97.4 grams, 492 mmoles) were added to a one liter one neck flask equipped with a magnetic stir bar and reflux condenser. The solution was placed under anhydrous nitrogen, stirred and heated to reflux for 16 hours. The reaction mixture was allowed to cool and was poured into one liter of hexanes. The solid was collected by suction filtration, washed with an additional 0.5 liters of hexanes, and dried under vacuum at room temperature to yield 45.5 grams (90%) of the title compound 1H NMR (400 MHz, DMSO-d6) δ: 11.86(s, 1H), 8.24(d, 1H), 6.84(d, 1H). ESI-MS m/z 308 (M+1).

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