Реакция #95260

ord-9547abe038d8402eb399bffdb459a63d

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONA stirred mixture of 380 g
  2. 2
    ДругоеThe cooled reaction mixture
  3. 3
    workup.ADDITIONis treated with 380 g
  4. 4
    Экстракцияof sodium carbonate and 2 liters of water and is extracted with ether
  5. 5
    ДругоеAcidic material is partitioned from the ether
  6. 6
    Экстракцияextract with 1.0 M sodium carbonate
  7. 7
    Экстракцияextracted with ether
  8. 8
    ПромывкаThe extract is washed successively with water and saturated sodium chloride
  9. 9
    Другоеdried
  10. 10
    Другоеevaporated
  11. 11
    Другоеto give an oil

Методика

A stirred mixture of 380 g. of mixed methyl and ethyl esters of 7-(2-carbethoxycyclohexan-1-on-2-yl)heptanoate (Example 10), 202 ml. of concentrated sulfuric acid, 970 ml. of glacial acetic acid, and 970 ml. of water is refluxed for 22.5 hours. The cooled reaction mixture is treated with 380 g. of sodium carbonate and 2 liters of water and is extracted with ether. Acidic material is partitioned from the ether extract with 1.0 M sodium carbonate. The aqueous phase is acidified with concentrated hydrochloric acid and extracted with ether. The extract is washed successively with water and saturated sodium chloride, dried, and evaporated to give an oil.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04343949uspto-grants-1982_08