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

HRID 1952576노트

반응식

HRID 1952576 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-f62d040622314b56a8afd72512183921
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08404859B2

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