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Water → 5-Cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-pyrazole

HRID 1194266
ノート
印刷プレビュー

反応式

HRID 1194266 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])=[CH:9][C:8]=2[Cl:18])[N:5]=[CH:4][CH:3]=1.N1C=CC=CC=1.[C:25]([CH2:27][C:28](Cl)=[O:29])#[N:26].O>C(#N)C>[C:25]([CH2:27][C:28]([NH:1][C:2]1[N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:16])([F:15])[F:17])=[CH:9][C:8]=2[Cl:18])[N:5]=[CH:4][CH:3]=1)=[O:29])#[N:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 110515942-Cyanoacetyl chlorideHCID 135571095-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole

生成物 1

HCID 139850675-Cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-pyrazole収率 80%

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

実験手順

22.5 g (0.076 mol) of 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole and 8 g (0.1 mol) of pyridine are taken in 200 ml of acetonitrile, and 13.2 g (0.128 mol) of cyanoacetyl chloride are added dropwise at 20°-25° C., while stirring and cooling. The reaction mixture is stirred at room temperature for a further two hours and then poured into water. After extraction with methylene chloride and drying of the organic phase over sodium sulphate, the solvent is distilled off in vacuo. The crystalline residue is stirred with a mixture of ligroin and diisopropyl ether and filtered off with suction. 22 g (80% of theory) of 5-cyanoacetylamino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-pyrazole of melting point 169°-175° C. are obtained.

後処理

  1. temperaturecooling
  2. stirringThe reaction mixture is stirred at room temperature for a further two hours
  3. extractionAfter extraction with methylene chloride
  4. dry with materialdrying of the organic phase over sodium sulphate
  5. distillationthe solvent is distilled off in vacuo
  6. stirringThe crystalline residue is stirred with a mixture of ligroin and diisopropyl ether
  7. filtrationfiltered off with suction

出典と根拠

ORDレコード
ord-766122a87d3147c59c59249c7b8aa355
出典データセット
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04814001

反応ノート

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