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Sodium Hydroxide → HCID 18317426、化合物

HRID 1700521
ノート
印刷プレビュー

反応式

HRID 1700521 の反応式
C([O:3][C:4]([C:6]1[C:10]2[C:11](=[O:21])[CH2:12][CH:13]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH2:14][C:9]=2[O:8][CH:7]=1)=[O:5])C.[OH-].[Na+]>C1COCC1>[C:4]([C:6]1[C:10]2[C:11](=[O:21])[CH2:12][CH:13]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH2:14][C:9]=2[O:8][CH:7]=1)([OH:5])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 183177573-Ethoxycarbonyl-6-phenyl-4,5,6,7-tetrahydrobenzofuran-4-one

生成物 1

HCID 18317426HCID 18317426、化合物収率 92.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

In THF (10 ml) was dissolved 3-ethoxycarbonyl-6-phenyl-4,5,6,7-tetrahydrobenzofuran-4-one (0.71 g). To the solution was added 1N sodium hydroxide (5.0 ml), and the mixture was stirred at room temperature overnight (12 hours). The reaction solution was concentrated under reduced pressure, and to the residue was added potassium hydrogensulfate to make the mixture acidic. To the mixture was added ethyl acetate, and the mixture was subjected to extraction. The upper layer was washed with saturated brine, dried (anhydrous magnesium sulfate) and concentrated under reduced pressure, and the residue was washed with isopropylether to give 3-carboxy-6-phenyl-4,5,6,7-tetrahydrobenzofuran-4-one (0.59 g).

後処理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. additionto the residue was added potassium hydrogensulfate
  3. additionTo the mixture was added ethyl acetate
  4. extractionthe mixture was subjected to extraction
  5. washThe upper layer was washed with saturated brine
  6. dry with materialdried (anhydrous magnesium sulfate)
  7. concentrationconcentrated under reduced pressure
  8. washthe residue was washed with isopropylether

出典と根拠

ORDレコード
ord-8694f1d6f9d1454e9a682b2f3ef91ec4
出典データセット
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06350749B1

反応ノート

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