Реакция #1152445

ord-7f5f7b648d794e73b873d9f1af68380a

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe reaction mixture is cooled
  2. 2
    Промывкаwashed successively with water, with a sodium hydroxide solution 5% and again with water
  3. 3
    Другоеdried
  4. 4
    Фильтрацияfiltered
  5. 5
    Другоеevaporated
  6. 6
    ДругоеThe residue is crystallized from 2-propanol

Методика

A mixture of 65 parts of 4-oxo-1-[4-(phenylmethoxy)phenyl]-1-cyclohexanecarbonitrile, 15.7 parts of 1,2-ethanediol, 0.2 parts of 4-methylbenzenesulfonic acid and 360 parts of methylbenzene is stirred and refluxed overnight with water-separator. The reaction mixture is cooled, washed successively with water, with a sodium hydroxide solution 5% and again with water, dried, filtered and evaporated. The residue is crystallized from 2-propanol, yielding 33.5 parts (47%) of 8-[4-(phenylmethoxy)phenyl]-1,4-dioxaspiro[4,5]decane-8-carbonitrile.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04329353uspto-grants-1982_05