Potassium Hydroxide → HCID 19904422、化合物

HRID 2372419ノート

反応式

HRID 2372419 の反応式
[C:1]([C:6]1([C:13](OCC)=[O:14])[CH2:11][CH2:10][CH2:9][CH2:8][C:7]1=[O:12])(OCC)=[O:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[K+].P([O-])([O-])(O)=O.[K+].[K+].P([O-])(O)(O)=O.[K+]>CCOCC.O>[OH:14][CH2:13][C:6]1([CH2:1][OH:2])[CH2:11][CH2:10][CH2:9][CH2:8][CH:7]1[OH:12]

参加物

8

反応物 5

HCID 14797Potassium HydroxideHCID 24450Potassium Phosphate, DibasicHCID 224023Diethyl 2-oxocyclohexane-1,1-dicarboxylateHCID 516951Monobasic potassium phosphateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 19904422HCID 19904422、化合物収率 60.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of 2,2-dicarbethoxycyclohexanone (3.0 g.) in dry ether (15 ml.) was added dropwise to a stirred suspension of lithium aluminium hydride (1.4 g.) in dry ether (50 ml.) at 0°, under nitrogen. The mixture was refluxed, with stirring, for six hours. Potassium hydroxide (6 g.) in water (100 ml) was added to the stirred mixture. Dipotassium hydrogen phosphate (4.2 g.) and potassium dihydrogen phosphate (3.3 g.) in water (50 ml.) was added. Ether was removed by passing a current of nitrogen through the mixture. The resultant slurry was acidified with glacial acetic acid and the solid was filtered off. The filtrate was evaporated in vacuo. The residue was extracted with acetone and the solution was evaporated in vacuo. 2,2Di-(hydroxymethyl)-cyclohexanol (1.2 g.) was obtained as a pale yellow oil.

後処理

  1. temperatureThe mixture was refluxed
  2. customEther was removed
  3. filtrationthe solid was filtered off
  4. customThe filtrate was evaporated in vacuo
  5. extractionThe residue was extracted with acetone
  6. customthe solution was evaporated in vacuo

出典と根拠

ORDレコード
ord-b58d505661ee43bc907e035160e47acb
出典データセット
uspto-grants-1992_03
特許番号
US05098929

反応ノート

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