반응 #79377

반응 방정식

4-fluoro-5-iodo-isatoic anhydride

formamidine acetate

→

title compound

수율 91.2%

4-Hydroxy-6-iodo-7-fluoroquinazoline

수율 91.2%

용매

Dimethylformamide

반응 조건

후처리

1. 1
   기타fitted with a magnetic stir bar
2. 2
   온도to cool
3. 3
   농축by concentrating the reaction mixture to one third its original volume
4. 4
   기타on the rotary evaporator
5. 5
   workup.ADDITIONThe resulting mixture was poured onto 3 liters of ice water
6. 6
   기타The resulting precipitated solid
7. 7
   여과was collected by suction filtration
8. 8
   세척The solid was washed with an additional one liter of distilled water
9. 9
   기타The resulting solid was dried under vacuum at 70° C.

실험 절차

Dimethylformamide (0.5 liters), 4-fluoro-5-iodo-isatoic anhydride (45 grams, 147 mmoles), and formamidine acetate (45.92 grams, 441 mmoles), were combined in a one liter one-neck flask fitted with a magnetic stir bar. The mixture was placed under anhydrous nitrogen and heated at 110° C. for 6 hours. The mixture was allowed to cool, followed by concentrating the reaction mixture to one third its original volume on the rotary evaporator. The resulting mixture was poured onto 3 liters of ice water. The resulting precipitated solid was collected by suction filtration. The solid was washed with an additional one liter of distilled water. The resulting solid was dried under vacuum at 70° C. to yield 38.9 grams (91%) of the title compound. 1H NMR (400 MHz, DMSO-d6) δ: 12.43(s, 1H), 8.46(d, 1H), 8.12(s, 1H), 7.49(d, 1H). ESI-MS m/z 291(M+1).

출처