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Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl ester → HCID 70435233、化合物

HRID 255675
ノート
印刷プレビュー

反応式

HRID 255675 の反応式
[CH:1]([C:3]1[N:4]([C:13]2[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][C:14]=2[CH3:20])[CH:5]=[C:6]([C:10](=[O:12])[CH:11]=1)[C:7]([OH:9])=[O:8])=O.[CH2:21]([O:23][C:24]([CH:26]=P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)=[O:25])[CH3:22]>CO>[CH2:21]([O:23][C:24]([CH:26]=[CH:1][C:3]1[N:4]([C:13]2[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][C:14]=2[CH3:20])[CH:5]=[C:6]([C:10](=[O:12])[CH:11]=1)[C:7]([OH:9])=[O:8])=[O:25])[CH3:22]
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 70670Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl esterHCID 14010769HCID 14010769、化合物

生成物 1

HCID 70435233HCID 70435233、化合物収率 32%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In 5 ml of methanol was dissolved 0.15 g of 6-formyl-1-(4-hydroxy-2-methylphenyl)-4-oxo-1,4-dihydronicotinic acid, and 0.19 g of ethoxycarbonylmethylenetriphenylphosphorane was added thereto. They were reacted at room temperature for one hour. After completion of the reaction, the solvent was removed by distillation under reduced pressure, and the residue was purified by a column chromatography (Wako Silica Gel C-200; eluent: chloroform/ethanol (50:1 by volume) mixture) to obtain 0.06 g of 6-(2-ethoxycarbonylethenyl)-1-(4-hydroxy-2-methylphenyl)-4-oxo-1,4-dihydronicotinic acid having a melting point of 185°-189° C.

後処理

  1. additionwas added
  2. customThey were reacted at room temperature for one hour
  3. customAfter completion of the reaction
  4. customthe solvent was removed by distillation under reduced pressure
  5. customthe residue was purified by a column chromatography (Wako Silica Gel C-200; eluent: chloroform/ethanol (50:1 by volume) mixture)

出典と根拠

ORDレコード
ord-da2cec772ee342b1b3e9048c7adbdfcb
出典データセット
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04698352

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