تفاعل #65432

معادلة التفاعل

ethyl 2,3-dibromo-1,4-benzodioxin-2-carboxylate

sodium iodide

→

Ethyl 1,4-benzodioxin-2-carboxylate

المردود 85.0%

المذيبات

acetone

ظروف التفاعل

المعالجة

1. 1
   تركيزThe reaction mixture is then concentrated under reduced pressure, hydrolysed with 80 cm3 of water
2. 2
   استخلاصsubsequently extracted with diethyl ether
3. 3
   تجفيفby drying over magnesium sulfate
4. 4
   تركيزthe ethereal phase is concentrated to dryness under reduced pressure
5. 5
   أخرىthe crude product is purified by chromatography on a silica column (eluant:petroleum ether/diethyl ether, 40:60)

الإجراء التجريبي

Stir for 3 hours, at room temperature and under a nitrogen atmosphere, a mixture of 16 g (43.7 mmol) of ethyl 2,3-dibromo-1,4-benzodioxin-2-carboxylate and 24 g (160 mmol) of sodium iodide in 80 cm3 of anhydrous acetone. The reaction mixture is then concentrated under reduced pressure, hydrolysed with 80 cm3 of water, and subsequently extracted with diethyl ether. After treatment with an aqueous sodium thiosulfate solution followed by drying over magnesium sulfate, the ethereal phase is concentrated to dryness under reduced pressure and the crude product is purified by chromatography on a silica column (eluant:petroleum ether/diethyl ether, 40:60). Ethyl 1,4-benzodioxin-2-carboxylate is thereby obtained in a yield of 85%.

المصدر