Реакция #6456

ord-8e967b2fdeb8454a83c24e9d3bcde951

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ПромывкаThe ethyl acetate solution is washed with H2O
  2. 2
    Другоеdried
  3. 3
    Концентрированиеconcentrated
  4. 4
    ДругоеPurification by column chromatography

Методика

5.6 g (0.04 mol) of 5,5-dimethyl-1,3-cyclohexanedione are dissolved in a mixture of 4.4 g (0.044 mol) of triethylamine and 120 ml of ethyl acetate. 8.7 g (0.044 mol) of benzothiadiazole-7-carboxylic acid chloride are added dropwise at 15° to 20° C., and the mixture is subsequently stirred overnight at room temperature. The ethyl acetate solution is washed with H2O, dried and concentrated. Purification by column chromatography using ethyl acetate/hexane gives 10.5 g (87.5%) of the title compound, melting point 131°-133° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05248683uspto-grants-1993_09