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

HRID 256729
ノート
印刷プレビュー

反応式

HRID 256729 の反応式
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]
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 3

HCID 176Acetic AcidHCID 14797Potassium HydroxideHCID 11745138HCID 11745138、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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),

後処理

  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

出典と根拠

ORDレコード
ord-d21c8bd49de84052b57ad91fd2ce93da
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05258529

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート