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Sulfuric Acid → 2-(4-Chlorophenyl)-5-trifluoromethylpyridazin-3-one

HRID 1421621
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HRID 1421621 반응식
S(=O)(=O)(O)O.[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([N:13]2[C:18](=[O:19])[CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[C:15](C(OCC)=O)=[N:14]2)=[CH:9][CH:8]=1>O>[Cl:6][C:7]1[CH:8]=[CH:9][C:10]([N:13]2[C:18](=[O:19])[CH:17]=[C:16]([C:20]([F:22])([F:21])[F:23])[CH:15]=[N:14]2)=[CH:11][CH:12]=1
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참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 1474610HCID 1474610, 화합물

생성물 1

HCID 110548972-(4-Chlorophenyl)-5-trifluoromethylpyridazin-3-one수율 45.4%

시약·촉매·용매 1

HCID 962Water용매2회

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온도
150 °C

실험 절차

Two mililiters (2 ml) of a mixture of sulfuric acid and water (v/v=1/1), and 0.5 g of 2-(4-chlorophenyl)-6-ethoxycarbonyl-5-trifluoromethylpyridazin-3-one (the present compound 1-51) were mixed and heated for 5 hours on a 150° C. oil bath. The reaction solution was cooled to room temperature, poured into water and extracted with 100 ml of ethyl acetate. The organic layer was washed with 50 ml of saturated sodium chloride solution twice and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure and the obtained crystals were washed with 50 ml of n-hexane to afford 0.18 g of 2-(4-chlorophenyl)-5-trifluoromethylpyridazin-3-one (yield:45%).

후처리

  1. temperatureThe reaction solution was cooled to room temperature
  2. extractionextracted with 100 ml of ethyl acetate
  3. washThe organic layer was washed with 50 ml of saturated sodium chloride solution twice
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was removed under reduced pressure
  6. washthe obtained crystals were washed with 50 ml of n-hexane

출처 및 근거

ORD 기록
ord-e754356bbc0344028efcbef956b64108
출처 데이터셋
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06077953

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