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Acetic Acid → 1-(2-Propynyl)cyclohexan-1-ol

HRID 259979
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반응식

HRID 259979 반응식
Cl[C:2](=[CH2:11])[CH2:3][C:4]1([OH:10])[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1.[OH-].[K+].C(O)(=O)C>CN(C)C=O>[CH2:3]([C:4]1([OH:10])[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1)[C:2]#[CH:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 14797Potassium HydroxideHCID 11745138HCID 11745138, 화합물

생성물 1

HCID 879381-(2-Propynyl)cyclohexan-1-ol

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

10.00 Grams of the 1-(2'-chloroallyl)-1-cyclohexanol obtained above were dissolved in 94 g of N,N-dimethylformamide, and 9.65 g of potassium hydroxide in a flake form were added. The mixture was stirred at room temperature for 6 hours, and neutralized with a 20% acetic acid aqueous solution. The resultant mixture was subjected to extraction with toluene. The toluene phase was washed with water and dried over magnesium sulfate. The desiccant was filtered off and the toluene was distilled off under reduced pressure to give 7.68 g of 1-propargyl-1-cyclohexanol; m.p.=53°-54° C., FI-MS m/e 138(M+) (Propargyl compound/allene compound=100.0/0.0),

후처리

  1. extractionThe resultant mixture was subjected to extraction with toluene
  2. washThe toluene phase was washed with water
  3. dry with materialdried over magnesium sulfate
  4. filtrationThe desiccant was filtered off
  5. distillationthe toluene was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-f374e7e5cef14f7889a6e8368c8174ec
출처 데이터셋
uspto-grants-1996_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05523495

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