Sodium Chloride → 5-(Methoxycarbonyl)-4-(trifluoromethyl)thiophene-2-carboxylic acid

HRID 1952576ノート

反応式

HRID 1952576 の反応式
[CH3:1][O:2][C:3]([C:5]1[S:6][C:7]([CH:14]=[O:15])=[CH:8][C:9]=1[C:10]([F:13])([F:12])[F:11])=[O:4].CC(=CC)C.[Cl-].[Na+].[O:23]1CCOCC1>O>[CH3:1][O:2][C:3]([C:5]1[S:6][C:7]([C:14]([OH:23])=[O:15])=[CH:8][C:9]=1[C:10]([F:11])([F:12])[F:13])=[O:4]

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 105532-Methyl-2-buteneHCID 312751,4-DioxaneHCID 71742491Methyl 5-formyl-3-(trifluoromethyl)-2-thiophenecarboxylate

生成物 1

HCID 682266025-(Methoxycarbonyl)-4-(trifluoromethyl)thiophene-2-carboxylic acid収率 100%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 5-Formyl-3-trifluoromethyl-thiophene-2-carboxylic acid methyl ester (2.05 g, 8.61 mmol) in dioxane (40 ml) was added 2-methyl-2-butene (9 ml) and a solution of Na2ClO2 (2.34 g, 25.92 mmol) and NaH2PO4 (2.82 g) in water (9 ml). The mixture was stirred at rt for 1.5 h. The solution was saturated with sodium chloride, then successively extracted with EtOAc. The combined organic layers were dried over Na2SO4 and concentrated under reduced pressure to afford the desired product (2.61 g, 100% yield).

後処理

  1. extractionsuccessively extracted with EtOAc
  2. dry with materialThe combined organic layers were dried over Na2SO4
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-f62d040622314b56a8afd72512183921
出典データセット
uspto-grants-2013_03
特許番号
US08404859B2

反応ノート

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