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Phosphorus oxide (P4O10) → Ethyl 4-(m-benzoylphenyl)-3-butenoate

HRID 1731177
ノート
印刷プレビュー

反応式

HRID 1731177 の反応式
O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[C:15]([C:23]1[CH:24]=[C:25]([CH2:29][CH:30](O)[CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33])[CH:26]=[CH:27][CH:28]=1)(=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>C1(C)C(C)=CC=CC=1>[C:15]([C:23]1[CH:24]=[C:25]([CH:29]=[CH:30][CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33])[CH:26]=[CH:27][CH:28]=1)(=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14812Phosphorus oxide (P4O10)HCID 21495623Ethyl 4-(m-benzoyl-phenyl)-3-hydroxybutyrate

生成物 1

HCID 53820247Ethyl 4-(m-benzoylphenyl)-3-butenoate

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

315 mg of phosphoric anhydride were added to a solution of 1.12 g of ethyl 4-(m-benzoyl-phenyl)-3-hydroxybutyrate in 20 ml of xylene and the mixture was refluxed for 2 hours and then cooled to room temperature. The organic phase was washed with water, then with an aqueous saturated sodium bicarbonate solution and then water, dried over sodium sulfate, treated with activated carbon, filtered and evaporated to dryness under reduced pressure. The residue was chromatographed over silica gel and was eluted with methylene chloride which was evaporated to dryness to obtain ethyl 4-(m-benzoylphenyl)-3-butenoate whose ultraviolet spectrum was in accord with the structure.

後処理

  1. temperaturethe mixture was refluxed for 2 hours
  2. washThe organic phase was washed with water
  3. dry with materialwith an aqueous saturated sodium bicarbonate solution and then water, dried over sodium sulfate
  4. additiontreated with activated carbon
  5. filtrationfiltered
  6. customevaporated to dryness under reduced pressure
  7. customThe residue was chromatographed over silica gel
  8. washwas eluted with methylene chloride which
  9. customwas evaporated to dryness

出典と根拠

ORDレコード
ord-291fe3ed4d4c4907883c4b2e0bd39110
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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