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Hydrochloric Acid → 6-fluoro-4-oxo-3,4-dihydro-2H-1-benzopyran-2-carboxylic acid

HRID 1111186
ノート
印刷プレビュー

反応式

HRID 1111186 の反応式
C(=O)(O)[O-].[Na+].[F:6][C:7]1[CH:8]=[CH:9][C:10]([OH:20])=[C:11]([C:13](=[O:19])/[CH:14]=[CH:15]/[C:16]([OH:18])=[O:17])[CH:12]=1.Cl>O>[F:6][C:7]1[CH:8]=[CH:9][C:10]2[O:20][CH:15]([C:16]([OH:18])=[O:17])[CH2:14][C:13](=[O:19])[C:11]=2[CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 145552584-(5-Fluoro-2-hydroxyphenyl)-4-oxobut-2-enoic acid

生成物 1

HCID 27785256-fluoro-4-oxo-3,4-dihydro-2H-1-benzopyran-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Sodium bicarbonate (2.10 g, 25.0 mmol) was added to a suspension of (E)-4-(5-fluoro-2-hydroxyphenyl)-4-oxo-2-butenoic acid (5.00 g, 23.8 mmol) (obtained through the process as described in Example 22) in 200 ml of distilled water and the mixture was refluxed for 10 minutes. After cooling, the reaction mixture was acidified to pH 1.0 with concentrated hydrochloric acid and then extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and evaporated in vacuo to give crude crystals which were recrystallized from the mixture of water and methanol to give 4.60 g (92.1%) of the subject desired compound as colorless crystals.

後処理

  1. customobtained through the process
  2. temperaturethe mixture was refluxed for 10 minutes
  3. temperatureAfter cooling
  4. extractionextracted with ethyl acetate
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. customevaporated in vacuo
  7. customto give crude crystals which
  8. customwere recrystallized from the mixture of water and methanol
  9. customto give 4.60 g (92.1%) of the

出典と根拠

ORDレコード
ord-721c77d1541143ffbe1b6431764c7e05
出典データセット
uspto-grants-1990_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04978758

反応ノート

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