تفاعل #1442521

معادلة التفاعل

thionyl bromide

pyridine

phenylmaleic anhydride

→

3-Bromo-4-phenylfuran-2,5-dione

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated at 75° C. for 30 min
2. 2
   درجة الحرارةto cool
3. 3
   أخرىexcess thionyl bromide was removed at 65° C. under reduced pressure
4. 4
   workup.STIRRINGThe mixture was then stirred with 150 ml of toluene
5. 5
   ترشيحfiltered
6. 6
   غسيلthe residue was washed twice with in each case 200 ml of toluene
7. 7
   تركيزthe filtrate was concentrated under reduced pressure
8. 8
   أخرىwas used without further purification

الإجراء التجريبي

At 10° C., first 40.2 g (193 mmol) of thionyl bromide and then 15.3 g (193 mmol) of pyridine were added dropwise with stirring to 16.8 g (97 mmol) of phenylmaleic anhydride in 200 ml of toluene. The mixture was stirred at 10° C. for 30 min, heated at 75° C. for 30 min using a preheated heating bath and allowed to cool, and excess thionyl bromide was removed at 65° C. under reduced pressure. The mixture was then stirred with 150 ml of toluene and filtered, and the residue was washed twice with in each case 200 ml of toluene, and the filtrate was concentrated under reduced pressure. The crude product (9.3 g) still contained 25% of unreacted starting material and was used without further purification.

المصدر