تفاعل #6919

معادلة التفاعل

4-fluoro-5-iodo-isatoic anhydride

formamidine acetate

→

title compound

المردود 91.2%

4-Hydroxy-6-iodo-7-fluoroquinazoline

المردود 91.2%

المذيبات

Dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   أخرىfitted with a magnetic stir bar
2. 2
   درجة الحرارةto cool
3. 3
   تركيزby concentrating the reaction mixture to one third its original volume
4. 4
   أخرىon the rotary evaporator
5. 5
   workup.ADDITIONThe resulting mixture was poured onto 3 litres of ice water
6. 6
   أخرىThe resulting precipitated solid
7. 7
   ترشيحwas collected by suction filtration
8. 8
   غسيلThe solid was washed with an additional one litre of distilled water
9. 9
   أخرىThe resulting solid was dried under vacuum at 70° C.

الإجراء التجريبي

Dimethylformamide (0.5 litres), 4-fluoro-5-iodo-isatoic anhydride (45 grams, 147 mmoles), and formamidine acetate (45.92 grams, 441 mmoles), were combined in a one litre 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 litres of ice water. The resulting precipitated solid was collected by suction filtration. The solid was washed with an additional one litre 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).

المصدر