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Acetic Anhydride → HCID 20465612, 화합물

HRID 328834
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HRID 328834 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 7918Acetic Anhydride2회HCID 521998p-Toluenesulfonic acid monohydrateHCID 204655182-(5-Hydroxypentyl)cyclopentan-1-oneHCID 867329372-(5-Hydroxypentyl)cyclopentanone 2-(5-acetoxypentyl)-cyclopentanone

생성물 1

HCID 20465612HCID 20465612, 화합물

실험 절차

A solution of 400 g. (2.04 moles) of a mixture of 2-(5-hydroxypentyl)cyclopentanone and 2-(5-acetoxypentyl)cyclopentanone (Example 70) 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 produce 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.

후처리

  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
  5. customto produce
  6. temperatureThe mixture is cooled
  7. custompartitioned between 2 l
  8. temperatureof cold water containing solid sodium bicarbonate to maintain a neutral pH
  9. washThe organic phase is washed with saturated brine
  10. dry with materialdried (MgSO4)
  11. customevaporated
  12. customto yield 452 g

출처 및 근거

ORD 기록
ord-23073027bc9f4efbbe648e977cfa3e32
출처 데이터셋
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04018811

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