Aluminium lithium hydride → (4-Methoxycyclohexyl)methanol

HRID 56895

反応式

HRID 56895 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][CH:9]1[CH2:14][CH2:13][CH:12]([C:15](OC)=[O:16])[CH2:11][CH2:10]1>C(OC)(C)(C)C>[CH3:7][O:8][CH:9]1[CH2:14][CH2:13][CH:12]([CH2:15][OH:16])[CH2:11][CH2:10]1

参加物

4

反応条件

温度
40 °C

実験手順

13.7 ml (27.5 mmol) of lithium aluminium hydride solution (2M in THF) was diluted with 82 ml of methyl tert-butyl ether, and a solution of 4.30 g (25.0 mmol) of methyl 4-methoxycyclohexanecarboxylate (cis/trans isomer mixture) in 82 ml of methyl tert-butyl ether was then added dropwise. The reaction solution was stirred at 40° C. for another 6 h and the reaction was then terminated by addition of 10 ml of water and 10 ml of aqueous 10% strength potassium hydroxide solution. The organic phase was decanted, dried over sodium sulphate and filtered, and the solvent was removed under reduced pressure. Yield: 3.24 g (90% of theory)

後処理

  1. customthe reaction was then terminated by addition of 10 ml of water and 10 ml of aqueous 10% strength potassium hydroxide solution
  2. customThe organic phase was decanted
  3. dry with materialdried over sodium sulphate
  4. filtrationfiltered
  5. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-0d53564daaef4c0d8e03d5230a61a068
出典データセット
uspto-grants-2016_09
特許番号
US09434690B2

関連ノート

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