반응 #2980

ord-0c37bb1656a64973bff4ef3e79448c12

반응 방정식

[H-]
hydride
[Al+3].[H-].[H-].[H-].[H-].[Li+]
lithium aluminum hydride
COC(=O)Cc1cccc2ccc(OC)cc12
methyl (7-methoxy-1-naphthyl)acetate
O
water
COc1ccc2cccc(CCO)c2c1
2-(7-METHOXY-1-NAPHTHYL)ETHANOL

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONare added slowly
  2. 2
    workup.WAITThe reaction medium is left
  3. 3
    workup.STIRRINGstirring for 30 minutes
  4. 4
    여과The reaction medium is filtered
  5. 5
    추출The aqueous phase is extracted with 3 times 50 cm3 of ether
  6. 6
    건조the ether phases are dried over magnesium sulfate
  7. 7
    기타evaporated
  8. 8
    기타The white solid obtained
  9. 9
    기타is recrystallized

실험 절차

3.34 g of lithium aluminum hydride are placed in a 250-cm3 flask, and ether is added gently with stirring. Using a dropping funnel, 5 g of methyl (7-methoxy-1-naphthyl)acetate previously dissolved in 50 cm3 of ether are added slowly. The reaction medium is left stirring for 30 minutes. It is poured very slowly into a mixture of water and ice so as to hydrolyze the excess unreacted hydride. The reaction medium is filtered. The aqueous phase is extracted with 3 times 50 cm3 of ether, and the ether phases are dried over magnesium sulfate and evaporated. The white solid obtained is recrystallized.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05731352uspto-grants-1998_03