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Potassium Hydroxide → 3,3-Di-(hydroxymethyl)-hexan-1-ol

HRID 704134
ノート
印刷プレビュー

反応式

HRID 704134 の反応式
C([O:3][C:4]([C:6]([CH2:18][CH2:19][CH3:20])([CH2:12][C:13](OCC)=[O:14])[C:7](OCC)=[O:8])=O)C.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[K+].P([O-])(O)(O)=O.[K+].P([O-])([O-])(O)=O.[K+].[K+]>CCOCC.O.C(O)(=O)C>[OH:3][CH2:4][C:6]([CH2:7][OH:8])([CH2:18][CH2:19][CH3:20])[CH2:12][CH2:13][OH:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 14797Potassium HydroxideHCID 24450Potassium Phosphate, DibasicHCID 516951Monobasic potassium phosphateHCID 20075591Diethyl 2-prop-1-yl-2-ethoxycarbonylsuccinateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 218851593,3-Di-(hydroxymethyl)-hexan-1-ol

試薬・触媒・溶媒

3
HCID 176Acetic Acid溶媒HCID 962Water溶媒HCID 3283Diethyl Ether溶媒2 回

実験手順

Diethyl 2-ethoxycarbonyl-2-n-propyl-succinate (55.8 g) in dry ether (50 ml.) was added slowly to a stirred suspension of lithium aluminium hydride (14.7 g.) in dry ether (150 ml.) at 0°, under a current of nitrogen. The mixture was stirred at room temperature for three hours and then refluxed, with stirring for four hours. A solution of potassium hydroxide (30.0 g.), potassium dihydrogen phosphate (22.0 g.) and potassium monohydrogen phosphate (22.0 g.) in water (200 ml.) was added to the cooled reaction mixture. The pH was adjusted to 5.0 with glacial acetic acid. The solid was removed by filtration and washed with water (40 ml.) The combined filtrates and washings were evaporated in vacuo. The residue was washed with acetone (3×100 ml). The acetone washings were evaporated in vacuo. The residue was washed with chloroform (3×100 ml.) and the washings were evaporated in vacuo, Toluene was added and the residue was evaporated in vacuo. 3,3-Di-(hydroxymethyl)-hexan-1-ol was obtained as a colourless oil and was used without further purification.

後処理

  1. temperaturerefluxed
  2. stirringwith stirring for four hours
  3. customThe solid was removed by filtration
  4. washwashed with water (40 ml.) The combined filtrates and washings
  5. customwere evaporated in vacuo
  6. washThe residue was washed with acetone (3×100 ml)
  7. customThe acetone washings were evaporated in vacuo
  8. washThe residue was washed with chloroform (3×100 ml.)
  9. customthe washings were evaporated in vacuo, Toluene
  10. additionwas added
  11. customthe residue was evaporated in vacuo

出典と根拠

ORDレコード
ord-45034e951f444a7ca2b9ba47e95e7606
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04985582

反応ノート

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