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

HRID 1952563노트

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HRID 1952563 반응식
[CH3:1][O:2][C:3]([C:5]1[S:6][C:7]([CH:11]=[O:12])=[CH:8][C:9]=1[CH3:10])=[O:4].CC(=CC)C.[Cl-].[Na+].[O:20]1CCOCC1>O>[CH3:1][O:2][C:3]([C:5]1[S:6][C:7]([C:11]([OH:20])=[O:12])=[CH:8][C:9]=1[CH3:10])=[O:4]

참가 물질

6

반응물 4

HCID 5234Sodium ChlorideHCID 105532-Methyl-2-buteneHCID 312751,4-DioxaneHCID 57618829Methyl 5-formyl-3-methylthiophene-2-carboxylate

생성물 1

HCID 682266195-(Methoxycarbonyl)-4-methylthiophene-2-carboxylic acid수율 90%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of 5-formyl-3-methyl-thiophene-2-carboxylic acid methyl ester (3.2 g, 17.4 mmol) in dioxane (20 ml) was added 2-methyl-2-butene (15 ml) and a solution of Na2ClO2 (4.71 g, 52.1 mmol) and NaH2PO4 (4.71 g, 39.2 mmol) in water (15 ml). The mixture was stirred at rt for 1 h. The solution was saturated with sodium chloride, then successively extracted with EtOAc and dichloromethane. The combined organic layers were dried over Na2SO4 and concentrated under reduced pressure to afford the desired product (3.13 g, 90% yield)

후처리

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

출처 및 근거

ORD 기록
ord-b8f669c751c148ecba9fdd0b9e2907e8
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08404859B2

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