反応 #65432

反応方程式

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

sodium iodide

→

Ethyl 1,4-benzodioxin-2-carboxylate

収率 85.0%

溶媒

acetone

反応条件

後処理

1. 1
   濃縮The reaction mixture is then concentrated under reduced pressure, hydrolysed with 80 cm3 of water
2. 2
   抽出subsequently extracted with diethyl ether
3. 3
   乾燥by drying over magnesium sulfate
4. 4
   濃縮the ethereal phase is concentrated to dryness under reduced pressure
5. 5
   その他the crude product is purified by chromatography on a silica column (eluant:petroleum ether/diethyl ether, 40:60)

実験手順

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%.

出典