Реакция #348711

ord-28adf486cf104b4d8d97dd240ed54f30

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураat reflux
  2. 2
    workup.STIRRINGThe reaction mixture is subsequently stirred
  3. 3
    Температураat reflux for 28 hours
  4. 4
    Температураcooled
  5. 5
    Фильтрацияfiltered
  6. 6
    Промывкаthe residue is washed with water/petroleum ether
  7. 7
    ЭкстракцияThe filtrate is extracted with petroleum ether
  8. 8
    Экстракцияthe petroleum ether extract
  9. 9
    Промывкаis washed with water
  10. 10
    Сушкаdried over sodium sulphate

Методика

335 g of zinc dust and 33.5 g of mercury (II) acetate and a solution of 330 cc of concentrated hydrochloric acid in 280 cc of water are rapidly added dropwise in a stirring apparatus. The mixture is boiled at reflux and a solution of 63 g of 2-ethyl-2-methyl-1-indanone in 525 cc of ethanol is added dropwise within 10 minutes while stirring. The reaction mixture is subsequently stirred at reflux for 28 hours, cooled, filtered, and the residue is washed with water/petroleum ether. The filtrate is extracted with petroleum ether, the petroleum ether extract is washed with water and dried over sodium sulphate. The crude 2-ethyl-2-methyl-indan, obtained as an oil after evaporating the solvent, is purified by chromatography on aluminium oxide/petroleum ether.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04166131uspto-grants-1979_08