Hydrochloric Acid → 2,4-DI-Tert-butylcyclohexanol

HRID 277317

反応式

HRID 277317 の反応式
[C:1]([CH:5]1[CH2:10][CH:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:8][CH2:7][C:6]1=[O:15])([CH3:4])([CH3:3])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].Cl>CCOCC>[C:1]([CH:5]1[CH2:10][CH:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:8][CH2:7][CH:6]1[OH:15])([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 114442Cyclohexanone, 2,4-bis(1,1-dimethylethyl)-HCID 21226445Aluminium lithium hydride

生成物 1

HCID 5460322,4-DI-Tert-butylcyclohexanol収率 88.1%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
23 °C

実験手順

380 g of 2,4-di-tert-butylcyclohexanone (mixed isomers) in 200 ml of ether are added dropwise with vigorous stirring to a suspension of 34.3 g (903 mmol) of lithium aluminium hydride in 1800 ml of ether over 4 hours, and the batch is subsequently stirred at 23° C. for 1 hour and admixed with 500 ml of 5% hydrochloric acid by vigorous stirring. The organic phase is separated off and washed twice with 250 ml of water each time. The organic phase is dried over MgSO4, evaporated and dried under reduced pressure to leave 337.80 g (88% of theory) of 2,4-di-tert-butylcyclohexanol (mixed isomers) as colourless wax.

後処理

  1. customThe organic phase is separated off
  2. washwashed twice with 250 ml of water each time
  3. dry with materialThe organic phase is dried over MgSO4
  4. customevaporated
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-8f6d695d03b5483caacc35b13a61e400
出典データセット
uspto-grants-2002_03
特許番号
US06355783B1

関連ノート

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