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

HRID 1779522노트

반응식

HRID 1779522 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-7eb4cd162ba74148a6d3aeeb79ea4d90
출처 데이터셋
uspto-grants-1997_05
특허 번호
US05627204

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