تفاعل #65439

ord-a34cd75a3c294cadabed2fc1ac5336bf

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزafter concentrating under reduced pressure
  2. 2
    استخلاصExtract with diethyl ether the acid which
  3. 3
    أخرىprecipitates
  4. 4
    أخرىafter drying
  5. 5
    تركيزconcentration to dryness
  6. 6
    غسيلwash the resulting acid with methylene chloride

الإجراء التجريبي

Under a nitrogen atmosphere, slowly add 75 mmol of a 10% aqueous sodium hydroxide solution to a solution of 2 g (7.5 mmol) of ethyl 7-acetoxy-2,3-dihydro-1,4-benzodioxin-2-carboxylate in 20 cm3 of methanol. Stir at room temperature for 6 hours and then, after concentrating under reduced pressure, acidify the mixture with a 2N hydrochloric acid solution. Extract with diethyl ether the acid which precipitates, then, after drying and concentration to dryness, wash the resulting acid with methylene chloride. 7-Hydroxy-2,3-dihydro-1,4-benzodioxin-2-carboxylic acid is thereby obtained in a yield of 85%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05420132uspto-grants-1995_05