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Acetic Anhydride → HCID 20453877、化合物

HRID 1462136
ノート
印刷プレビュー

反応式

HRID 1462136 の反応式
[NH2:1][C:2]1[N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:17])([F:16])[F:15])=[C:9]([Cl:18])[C:8]=2[Cl:19])[N:5]=[CH:4][C:3]=1[C:20]#[N:21].[C:22](OC(=O)C)(=[O:24])[CH3:23]>O>[C:22]([NH:1][C:2]1[N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:17])([F:15])[F:16])=[C:9]([Cl:18])[C:8]=2[Cl:19])[N:5]=[CH:4][C:3]=1[C:20]#[N:21])(=[O:24])[CH3:23]
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 7918Acetic AnhydrideHCID 13122001HCID 13122001、化合物

生成物 1

HCID 20453877HCID 20453877、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

5-Amino-4-cyano-1-(2,3,6-trichloro-4-trifluoromethylphenyl)pyrazole (3.74 g) in acetic anhydride (20 ml) was heated at reflux for 6 hours. The reaction mixture was then evaporated under reduced pressure to remove unreacted acetic anhydride. The residual oil was dissolved in dichloromethane (50 ml) and filtered. The filtrate was evaporated to give a foam, which was then suspended in water (70 ml). The suspension was filtered and the filtrate deposited a solid on standing. The solid was collected by filtration and washed with water to give 5-acetamido-4-cyano-1-(2,3,6-trichloro-4-trifluoromethylphenyl)pyrazole (0.4 g), m.p. 177°-178° C., in the form of a fawn-coloured solid.

後処理

  1. temperatureat reflux for 6 hours
  2. customThe reaction mixture was then evaporated under reduced pressure
  3. customto remove unreacted acetic anhydride
  4. dissolutionThe residual oil was dissolved in dichloromethane (50 ml)
  5. filtrationfiltered
  6. customThe filtrate was evaporated
  7. customto give a foam, which
  8. filtrationThe suspension was filtered
  9. filtrationThe solid was collected by filtration
  10. washwashed with water

出典と根拠

ORDレコード
ord-0fbe4585ccd74e27bdad730164787c32
出典データセット
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04459150

反応ノート

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