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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Methyl iodide → HCID 13066681, 화합물

HRID 1164001
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HRID 1164001 반응식
[OH:1][C:2]1[C:7]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[Cl:15])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:16][C:17]([OH:19])=[O:18].CI.[C:22](=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:22][O:1][C:2]1[C:7]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[Cl:15])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:16][C:17]([OH:19])=[O:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 130666802-[2-Hydroxy-3-(2-chlorophenoxy)phenyl]acetic acid

생성물 1

HCID 13066681HCID 13066681, 화합물수율 67.6%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 2-[2-hydroxy-3-(2-chlorophenoxy)phenyl]acetic acid (1.9 g), methyl iodide (2.3 g) and potassium carbonate (2.2 g) in acetone (40 ml) was refluxed under heating for 4.5 hrs. After cooling, the reaction mixture was filtered. The filtrate was evaporated, and the oily residue was dissolved in methanol (30 ml). To the solution was added potassium hydroxide (1 g), and the mixture was refluxed under heating for 30 minutes. After cooling, the reaction mixture was evaporated and the residue was dissolved in water. The aqueous solution was washed with diethyl ether, acidified with conc. hydrochloric acid and extracted with diethyl ether. The extract was washed with water, dried over magnesium sulfate and evaporated. The residue was recrystallized from a mixture of benzene and n-hexane to give 2-[2-methoxy-3-(2-chlorophenoxy)phenyl]acetic acid (1.35 g). mp 87°-92° C.

후처리

  1. temperaturewas refluxed
  2. temperatureunder heating for 4.5 hrs
  3. temperatureAfter cooling
  4. filtrationthe reaction mixture was filtered
  5. customThe filtrate was evaporated
  6. dissolutionthe oily residue was dissolved in methanol (30 ml)
  7. additionTo the solution was added potassium hydroxide (1 g)
  8. temperaturethe mixture was refluxed
  9. temperatureunder heating for 30 minutes
  10. temperatureAfter cooling
  11. customthe reaction mixture was evaporated
  12. dissolutionthe residue was dissolved in water
  13. washThe aqueous solution was washed with diethyl ether
  14. extractionextracted with diethyl ether
  15. washThe extract was washed with water
  16. dry with materialdried over magnesium sulfate
  17. customevaporated
  18. customThe residue was recrystallized from a mixture of benzene and n-hexane

출처 및 근거

ORD 기록
ord-401cb9a9f30b495faad6c359e36ca6de
출처 데이터셋
uspto-grants-1983_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04367238

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