Sodium Hydroxide → 5-Chlorofuran-2-carboxylic acid

HRID 357783

反応式

HRID 357783 の反応式
C([O:3][C:4]([C:6]1[O:7][C:8]([Cl:11])=[CH:9][CH:10]=1)=[O:5])C.[OH-].[Na+]>C(O)C>[Cl:11][C:8]1[O:7][C:6]([C:4]([OH:5])=[O:3])=[CH:10][CH:9]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 11137631Ethyl 5-chlorofuran-2-carboxylate

生成物 1

HCID 2348535-Chlorofuran-2-carboxylic acid収率 78.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

5-Chloro-2-furancarboxylic acid ethyl ester (8 g) (synthesized in accordance with the method described in Chem. Pharm. Bull., 40, 1966 (1992)) was dissolved in ethanol (50 ml), and 1N aqueous sodium hydroxide (50 ml) was added. The mixture was stirred at room temperature for 1 hour and concentrated under reduced pressure. The residue was dissolved in water and washed with diethyl ether. The aqueous layer was acidified with 1N hydrochloric acid and extracted with ethyl acetate. The extract was washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. Precipitated crystals were collected by filtration and washed with diethyl etherhexane to give 5-chloro-2-furancarboxylic acid (5.3 g) as crystals.

後処理

  1. concentrationconcentrated under reduced pressure
  2. dissolutionThe residue was dissolved in water
  3. washwashed with diethyl ether
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with water and saturated aqueous sodium chloride
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customPrecipitated crystals
  9. filtrationwere collected by filtration
  10. washwashed with diethyl etherhexane

出典と根拠

ORDレコード
ord-14bf8d6b55f04ff9ab631075257b51ca
出典データセット
uspto-grants-1998_11
特許番号
US05840917

関連ノート

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