反应 #2980

ord-0c37bb1656a64973bff4ef3e79448c12

反应方程式

[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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONare added slowly
  2. 2
    workup.WAITThe reaction medium is left
  3. 3
    workup.STIRRINGstirring for 30 minutes
  4. 4
    过滤The reaction medium is filtered
  5. 5
    萃取The aqueous phase is extracted with 3 times 50 cm3 of ether
  6. 6
    干燥the ether phases are dried over magnesium sulfate
  7. 7
    其他evaporated
  8. 8
    其他The white solid obtained
  9. 9
    其他is recrystallized

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05731352uspto-grants-1998_03