Hydrochloric Acid → 4-Iodo-2-methoxyphenol

HRID 1532987노트

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HRID 1532987 반응식
[C:1]1([O:8][CH3:9])[C:2](=[CH:4][CH:5]=[CH:6][CH:7]=1)[OH:3].[I-:10].[Na+].[OH-].[Na+].Cl[O-].[Na+].Cl.S([O-])([O-])=O.[Na+].[Na+]>CO>[I:10][C:6]1[CH:5]=[CH:4][C:2]([OH:3])=[C:1]([O:8][CH3:9])[CH:7]=1

참가 물질

8

반응물 6

HCID 313Hydrochloric AcidHCID 460GuaiacolHCID 5238Sodium IodideHCID 14798Sodium HydroxideHCID 24437Sodium SulfiteHCID 23665760Sodium Hypochlorite

생성물 1

HCID 101061274-Iodo-2-methoxyphenol

시약·촉매·용매 1

HCID 887Methanol용매

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온도
0 °C

실험 절차

4-Iodo-2-methoxyphenol was prepared according to the method described by K. J. Edgar and N. Falling, J. Org. Chem. 55, 5287 (1990). Guaiacol (50.0 g, 402 mmol), sodium iodide (60.5 g, 402 mmol) was dissolved in methanol (800 ml) and cooled to 0° C., and sodium hydroxide (16.0 g, 402 mmol) was added at such a rate that the temperature did not exceed 5° C. An aqueous solution of sodium hypochlorite (750 ml, 7.2% solution, 402 mmol) was added during 45 min. The temperature was not allowed to exceed 0° C. After completed addition it was stirred for another 10 minutes at 0° C. First aqueous hydrochloric acid (100 ml, 4 M solution) and then sodium sulfite (200 ml saturated aqueous solution) was added. The product was extracted with ether was followed by drying over magnesium sulfate. Evaporation of the solvent was followed by distillation and the fraction at 105-106° C. at 0.1 mm Hg was collected. Yield 55 g, 54%.

후처리

  1. customdid not exceed 5° C
  2. customto exceed 0° C
  3. additionaddition it
  4. extractionThe product was extracted with ether
  5. dry with materialby drying over magnesium sulfate
  6. customEvaporation of the solvent
  7. distillationwas followed by distillation
  8. customthe fraction at 105-106° C. at 0.1 mm Hg was collected

출처 및 근거

ORD 기록
ord-9616f72f78e54859bf28459a527921b4
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06207662B1

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