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Acetic Acid → 5-Chloro-6-(2-methylphenoxy)-3-pyridazinol

HRID 1821681
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인쇄 미리보기

반응식

HRID 1821681 반응식
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]=[N:4][C:3]=1[O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH3:16].C(O)(=[O:19])C.C([O-])(=O)C.[K+]>O>[Cl:1][C:2]1[CH:7]=[C:6]([OH:19])[N:5]=[N:4][C:3]=1[O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 517044Potassium AcetateHCID 23013971HCID 23013971, 화합물

생성물 1

HCID 1784243955-Chloro-6-(2-methylphenoxy)-3-pyridazinol수율 85.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture comprising 578 mg (2.27 mmol) of 4,6-dichloro-3-(2-methylphenoxy)pyridazine obtained in Example 1 (2), acetic acid (10 mL) and 0.45 g (4.6 mmol) of potassium acetate was refluxed for 5 hours. The reaction mixture was allowed to stand for cooling, and after adding 50 mL of water, the mixture was extracted with ethyl acetate. The organic layers were combined, and washed successively with water and brine. After drying over anhydrous sodium sulfate, the solvent was removed to obtain 461 mg (1.95 mmol, Yield: 85.9%) of 5-chloro-6-(2-methylphenoxy)-3-pyridazinol.

후처리

  1. temperaturefor cooling
  2. extractionthe mixture was extracted with ethyl acetate
  3. washwashed successively with water and brine
  4. dry with materialAfter drying over anhydrous sodium sulfate
  5. customthe solvent was removed

출처 및 근거

ORD 기록
ord-a06722ce6e724bbab1669621691045c8
출처 데이터셋
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07608563B2

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