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Potassium Hydroxide → HCID 178526870、化合物

HRID 622291
ノート
印刷プレビュー

反応式

HRID 622291 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[N:10]1[C:14](Cl)=[C:13]([N+:16]([O-:18])=[O:17])[CH:12]=[N:11]1.[OH-:19].[K+]>CO>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[N:10]1[C:14]([OH:19])=[C:13]([N+:16]([O-:18])=[O:17])[CH:12]=[N:11]1
参加物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 14797Potassium Hydroxide2 回HCID 136896085-Chloro-4-nitro-1-(2,4,6-trichlorophenyl)-1H-pyrazole

生成物 1

HCID 178526870HCID 178526870、化合物収率 49%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3.3 g of 1-(2,4,6-trichlorophenyl)-4-nitro-5-chloropyrazole are suspended in 10 ml of methanol, and 20 ml of 1N methanolic potassium hydroxide solution are added. The mixture is refluxed for 12 hours. In order to achieve complete reaction, a further 10 ml of 1N methanolic potassium hydroxide solution are added to the reaction mixture, which is refluxed for a further 12 hours. For work-up, the mixture is filtered, the solvent is stripped off in vacuo, the residue is taken up in hot water, and the product is precipitated by acidification with 2N hydrochloric acid. After filtering off and drying, 1.5 g (49% of theory) of 1-(2,4,6-trichlorophenyl)-4-nitro-5-hydroxypyrazole of melting point 106°-115° C. are obtained.

後処理

  1. temperatureThe mixture is refluxed for 12 hours
  2. customreaction
  3. temperatureis refluxed for a further 12 hours
  4. filtrationFor work-up, the mixture is filtered
  5. customthe product is precipitated by acidification with 2N hydrochloric acid
  6. filtrationAfter filtering off
  7. customdrying

出典と根拠

ORDレコード
ord-82ca9ed688b44acfb09b731e9d104103
出典データセット
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04770692

反応ノート

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