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

HRID 441056노트

반응식

HRID 441056 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 of 32 mg of 5,7-dihydroxy-2-methylsulfinylchromone (0.134 mmol), 20 mg of 4-hydroxybenzenethiol (0.161 mmol), 41 mg of potassium carbonate (0. 295 mmol) and 2 ml acetone was stirred overnight at room temperature. The reaction solution was neutralized with dilute hydrochloric acid and then extracted twice with ethyl acetate. The organic layer was washed with saturated NaCl water and dried over sodium sulfate anhydride. The solvent was distilled off under reduced pressure, and the crude product was subjected to recrystallization from acetone-hexane, to give 14.6 mg of 5,7-dihydroxy-2-(4-hydroxyphenylthio)chromone (36% yield).

후처리

  1. extractionextracted twice with ethyl acetate
  2. washThe organic layer was washed with saturated NaCl water
  3. dry with materialdried over sodium sulfate anhydride
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe crude product was subjected to recrystallization from acetone-hexane

출처 및 근거

ORD 기록
ord-0d726f084be9443a8d4285eff3c513d6
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05521216

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