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Methyl 4-oxo-4-(4-phenoxyphenyl)but-2-enoate → HCID 13276507、化合物

HRID 2418151
ノート
印刷プレビュー

反応式

HRID 2418151 の反応式
[O:1]([C:8]1[CH:21]=[CH:20][C:11]([C:12]([CH:14]=[CH:15][C:16]([O:18][CH3:19])=[O:17])=[O:13])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:22]([OH:25])(=[S:24])[CH3:23]>C(OCC)C>[C:22]([S:24][CH:15]([CH2:14][C:12](=[O:13])[C:11]1[CH:20]=[CH:21][C:8]([O:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[CH:9][CH:10]=1)[C:16]([O:18][CH3:19])=[O:17])(=[O:25])[CH3:23]
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 53908224Methyl 4-oxo-4-(4-phenoxyphenyl)but-2-enoateHCID 178418634HCID 178418634、化合物

生成物 1

HCID 13276507HCID 13276507、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

2.82 g of methyl 3-(4-phenoxybenzoyl)acrylate were dissolved in 30 ml of diethyl ether, then 1.5 ml of thioacetic acid were added. The mixture was stirred for 3 hours. The reaction mixture was washed, in turn, with water, a saturated aqueous solution of sodium hydrogencarbonate and water and then dried over magnesium sulfate. The diethyl ether was removed by distillation under reduced pressure. The residue was purified first by silica gel column chromatography, eluted with a mixture of hexane and diethyl ether, then by recrystallization from a mixture of hexane and diethyl ether to give 2.91 g of methyl 2-acetylthio-3-(4-phenoxybenzoyl)-propionate.

後処理

  1. washThe reaction mixture was washed, in turn, with water
  2. dry with materiala saturated aqueous solution of sodium hydrogencarbonate and water and then dried over magnesium sulfate
  3. customThe diethyl ether was removed by distillation under reduced pressure
  4. customThe residue was purified first by silica gel column chromatography
  5. washeluted with a mixture of hexane and diethyl ether
  6. customby recrystallization
  7. additionfrom a mixture of hexane and diethyl ether

出典と根拠

ORDレコード
ord-5b703ee12b9a4357846b23280ce89c7a
出典データセット
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04472316

反応ノート

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