Hydrochloric Acid → 5,7-Dihydroxy-2-(4-hydroxyphenylthio)chromone

HRID 1779522ノート

反応式

HRID 1779522 の反応式
[OH:1][C:2]1[CH:11]=[C:10]([OH:12])[CH:9]=[C:8]2[C:3]=1[C:4](=[O:16])[CH:5]=[C:6]([S:13]([CH3:15])=O)[O:7]2.[OH:17][C:18]1[CH:23]=[CH:22]C(S)=[CH:20][CH:19]=1.C(=O)([O-])[O-].[K+].[K+].Cl>CC(C)=O>[OH:1][C:2]1[CH:11]=[C:10]([OH:12])[CH:9]=[C:8]2[C:3]=1[C:4](=[O:16])[CH:5]=[C:6]([S:13][C:15]1[CH:22]=[CH:23][C:18]([OH:17])=[CH:19][CH:20]=1)[O:7]2

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 2401474-MercaptophenolHCID 229064885,7-Dihydroxy-2-methylsulfinylchromone

生成物 1

HCID 229064625,7-Dihydroxy-2-(4-hydroxyphenylthio)chromone収率 36%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture consisting of 32 mg (0.134 mmol) 5,7-dihydroxy-2-methylsulfinylchromone, 20 mg (0.161 mmol) 4-hydroxybenzenethiol, 41 mg (0.295 mmol) potassium carbonate, and 2 ml acetone was stirred overnight at room temperature. The solution thus reacted was neutralized by addition of dilute hydrochloric acid. Subsequently, the product was extracted twice with ethyl acetate. The organic layer was washed with brine and dried over anhydrous sodium sulfate. The solvent was distilled out under reduced pressure. The resulting crude product was subjected to recrystallization from acetone-hexane, whereby 14.6 mg of 5,7-dihydroxy-2-(4-hydroxyphenylthio)chromone was obtained (yield: 36%).

後処理

  1. customThe solution thus reacted
  2. extractionSubsequently, the product was extracted twice with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled out under reduced pressure
  6. customThe resulting crude product was subjected to recrystallization from acetone-hexane

出典と根拠

ORDレコード
ord-7eb4cd162ba74148a6d3aeeb79ea4d90
出典データセット
uspto-grants-1997_05
特許番号
US05627204

反応ノート

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