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Acetic Anhydride → HCID 20465612、化合物

HRID 66973
ノート
印刷プレビュー

反応式

HRID 66973 の反応式
[OH:1][CH2:2][CH2:3]CCCC1CCCC1=O.OCCCCCC1CCCC1=O.[C:25]([O:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH:34]1[CH2:38][CH2:37][CH2:36][C:35]1=[O:39])(=[O:27])[CH3:26].O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(OC(=O)C)(=O)C>>[C:2]([O:39][C:35]1[CH2:36][CH2:37][CH2:38][C:34]=1[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29][O:28][C:25](=[O:27])[CH3:26])(=[O:1])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 7918Acetic Anhydride2 回HCID 521998p-Toluenesulfonic acid monohydrateHCID 204655182-(5-Hydroxypentyl)cyclopentan-1-oneHCID 867329372-(5-Hydroxypentyl)cyclopentanone 2-(5-acetoxypentyl)-cyclopentanone

生成物 1

HCID 20465612HCID 20465612、化合物

実験手順

A solution of 400 g. (2.04 moles) of a mixture of 2-(5-hydroxypentyl)cyclopentanone and 2-(5-acetoxypentyl)cyclopentanone (Example 55) and 4.0 g. of p-toluenesulfonic acid monohydrate in 1 l. of acetic anhydride is refluxed at a rate to maintain a steady distillation of acetic acid from the reaction through a helix-packed fractionation column. The reaction is continued with the addition of acetic anhydride to maintain a constant volume until complete conversion of starting materials to product is evident. The mixture is cooled and partitioned between 2 l. of hexane and 3 l. of cold water containing solid sodium bicarbonate to maintain a neutral pH. The organic phase is washed with saturated brine. dried (MgSO4), and evaporated to yield 452 g. of an oil.

後処理

  1. temperatureto maintain
  2. distillationa steady distillation of acetic acid
  3. customfrom the reaction through a helix-packed fractionation column
  4. temperatureto maintain a constant volume until complete conversion of starting materials to product
  5. temperatureThe mixture is cooled
  6. custompartitioned between 2 l
  7. temperatureof cold water containing solid sodium bicarbonate to maintain a neutral pH
  8. washThe organic phase is washed with saturated brine
  9. dry with materialdried (MgSO4)
  10. customevaporated
  11. customto yield 452 g

出典と根拠

ORDレコード
ord-4f2359555168413fb3d83b5c45b8f9c5
出典データセット
uspto-grants-1982_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04343949

反応ノート

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