Nitric Acid → 5-Cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-4-nitro-pyrazole

HRID 622607ノート

反応式

HRID 622607 の反応式
[C:1]([CH2:3][C:4]([NH:6][C:7]1[N:11]([C:12]2[C:17]([Cl:18])=[CH:16][C:15]([C:19]([F:22])([F:21])[F:20])=[CH:14][C:13]=2[Cl:23])[N:10]=[CH:9][CH:8]=1)=[O:5])#[N:2].C(OC(=O)C)(=O)C.[N+:31]([O-])([OH:33])=[O:32]>C(O)(=O)C>[C:1]([CH2:3][C:4]([NH:6][C:7]1[N:11]([C:12]2[C:17]([Cl:18])=[CH:16][C:15]([C:19]([F:20])([F:22])[F:21])=[CH:14][C:13]=2[Cl:23])[N:10]=[CH:9][C:8]=1[N+:31]([O-:33])=[O:32])=[O:5])#[N:2]

参加物

5

反応物 3

HCID 944Nitric AcidHCID 7918Acetic AnhydrideHCID 139850675-Cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-pyrazole

生成物 1

HCID 139850685-Cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-4-nitro-pyrazole収率 36%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

7.26 g (0.02 mol) of 5-cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-pyrazole (Example 1) are taken in 70 ml of glacial acetic acid, and 2 ml of acetic anhydride and 2 ml of nitric acid are added dropwise in succession at about 10° C. A crystalline solid precipitates out of the initially clear solution after prolonged stirring. After filtration with suction, washing several times with diisopropyl ether and drying, 2.9 g (36% of theory) of 5-cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-4-nitro-pyrazole of melting point 221°-223° C. are obtained.

後処理

  1. customA crystalline solid precipitates out of the initially clear solution
  2. filtrationAfter filtration with suction
  3. washwashing several times with diisopropyl ether
  4. customdrying

出典と根拠

ORDレコード
ord-66cb4facf573415587a386fcd5e8c7cc
出典データセット
uspto-grants-1988_09
特許番号
US04772310

反応ノート

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