반응 #6608

ord-8d935727faf84d70b9ee58a54f250c2e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도under reflux for 3 h
  2. 2
    온도cooled
  3. 3
    추출The mixture was extracted three times with ether
  4. 4
    세척the combined ether extracts were washed with water
  5. 5
    건조dried over Na2SO4
  6. 6
    농축concentrated

실험 절차

A suspension of 3 g (9.4 mmol) of 4-cyanobenzyl 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl ether in 60 ml of ether was added dropwise under nitrogen to a suspension of 1 g (26 mmol) of lithium aluminum hydride in 50 ml of dry ether at 25° C. The mixture was then stirred under reflux for 3 h, cooled and hydrolyzed cautiously with water and sodium sulfate solution. The mixture was extracted three times with ether, and the combined ether extracts were washed with water, dried over Na2SO4 and concentrated. 3 g of the title compound of melting point 77°-79° C. remained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05248823uspto-grants-1993_09