6-nitro-4H-1,3-benzodioxine → HCID 56975056, compound

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Reaction Steps

30 g(0.17 Mol) 6-Nitro-1,3-benzodioxan III are dissolved in 300 ml of certain alcohols. After addition of 15 ml of water 60 ml concentrated sulfuric acid is added dropwise with stirring. The solution is heated under reflux until completely converted to product with the help of a control by thin layer chromatography. After cooling the reaction mixture is mixed with about 200 ml water and the solution is concentrated to about 1/3 of its volume under vacuum. A yellow oil comes down which is extracted with ether. The ether phase is dried by sodium sulfate and the residue is filtered by silica gel with methylene chloride as elution agent. After concentration of the methylene chloride solution light yellow crystals of the corresponding 4-nitrophenol compound precipitate.

Provenance & Evidence