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Sodium Hydroxide → 3,5-Dimethoxybenzofuran-2-carboxylic acid

HRID 256345
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HRID 256345 반응식
[CH3:1][O:2][C:3]1[C:7]2[CH:8]=[C:9]([O:12][CH3:13])[CH:10]=[CH:11][C:6]=2[O:5][C:4]=1[C:14]([O:16]C)=[O:15].[OH-].[Na+]>CO>[CH3:1][O:2][C:3]1[C:7]2[CH:8]=[C:9]([O:12][CH3:13])[CH:10]=[CH:11][C:6]=2[O:5][C:4]=1[C:14]([OH:16])=[O:15]
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 13682649HCID 13682649, 화합물

생성물 1

HCID 136826533,5-Dimethoxybenzofuran-2-carboxylic acid수율 96%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 10.6 g (0.045 mole) of 3,5-dimethoxy-2 -benzofurancarboxylic acid, methyl ester in 80 ml of methanol is treated with 75 ml of 1.0 N aqueous sodium hydroxide solution. The new mixture is stirred at reflux for 45 minutes, cooled, and added to 750 g of ice/water. After extraction with dichloromethane, 3×300 ml) the aqueous layer is cooled in ice and acidified with glacial acetic acid to precipitate the crude product. The precipitate is filtered and washed with water to yield 9.6 g (88% crude yield) of 3,5-dimethoxy-2-benzofurancarboxylic acid. A sample recrystallized from ethyl acetate is analytically pure, mp 168° C.-dec.

후처리

  1. temperatureat reflux for 45 minutes
  2. temperaturecooled
  3. extractionAfter extraction with dichloromethane, 3×300 ml) the aqueous layer
  4. temperatureis cooled in ice
  5. customto precipitate the crude product
  6. filtrationThe precipitate is filtered
  7. washwashed with water

출처 및 근거

ORD 기록
ord-ca4fddc7abee41a4801902f291214cbd
출처 데이터셋
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04703053

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