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Ethanol → HCID 54538359、化合物

HRID 1731178
ノート
印刷プレビュー

反応式

HRID 1731178 の反応式
[C:1]([C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH2:17][C:18]([O:20]CC)=[O:19])[CH:12]=[CH:13][CH:14]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(O)C.[OH-].[K+]>O>[C:1]([C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH2:17][C:18]([OH:20])=[O:19])[CH:12]=[CH:13][CH:14]=1)(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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 702Ethanol2 回HCID 14797Potassium HydroxideHCID 53820247Ethyl 4-(m-benzoylphenyl)-3-butenoate

生成物 1

HCID 54538359HCID 54538359、化合物収率 66.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 275 mg of ethyl 4-(m-benzoyl-phenyl)-3-butenoate, 2.75 ml of ethanol, 0.275 ml of ethanol, 0.275 ml of water and 0.08 ml of 12.5N potassium hydroxide was refluxed for 30 minutes and then was evaporated to dryness. The residue was dissolved in 10 ml of water and the solution was treated with activated carbon, and filtered. 3 ml of N hydrochloric acid were added thereto and the mixture was extracted with methylene chloride. The organic phase was washed with water, dried over sodium sulfate, treated with activated carbon, filtered and evaporated to dryness under reduced pressure to obtain 166 mg of 4-(m-benzoyl-phenyl)-3-butenoic acid in the form of a yellow oil soluble in chloroform and ethanol and insoluble in water.

後処理

  1. temperaturewas refluxed for 30 minutes
  2. customwas evaporated to dryness
  3. dissolutionThe residue was dissolved in 10 ml of water
  4. additionthe solution was treated with activated carbon
  5. filtrationfiltered
  6. addition3 ml of N hydrochloric acid were added
  7. extractionthe mixture was extracted with methylene chloride
  8. washThe organic phase was washed with water
  9. dry with materialdried over sodium sulfate
  10. additiontreated with activated carbon
  11. filtrationfiltered
  12. customevaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-ede664cd509e4f3eb9d69638206814dd
出典データセット
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03995056

反応ノート

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