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

HRID 1421621
ノート
印刷プレビュー

反応式

HRID 1421621 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 1474610HCID 1474610、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
150 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-e754356bbc0344028efcbef956b64108
出典データセット
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06077953

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート