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Hydrazine hydrate (1:1) → 2,3-Dichloro-4-trifluoromethyl-phenylhydrazine

HRID 34861
ノート
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反応式

HRID 34861 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[C:6](Cl)[CH:5]=[CH:4][C:3]=1[C:10]([F:13])([F:12])[F:11].O.[NH2:15][NH2:16]>N1C=CC=CC=1>[Cl:8][C:7]1[C:2]([Cl:1])=[C:3]([C:10]([F:13])([F:12])[F:11])[CH:4]=[CH:5][C:6]=1[NH:15][NH2:16]
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 24654Hydrazine hydrate (1:1)HCID 133082441,2,3-Trichloro-4-(trifluoromethyl)benzene

生成物 1

HCID 139134182,3-Dichloro-4-trifluoromethyl-phenylhydrazine収率 79.4%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

100 g of 2,3,4-trichlorobenzotrifluoride are initially introduced, 200 ml of pyridine are added, followed by 100 g of hydrazine hydrate and the mixture is then heated to the reflux temperture for 12 hours. Thereafter, 90% of the pyridine is distilled off and the remaining residue is stirred into 250 ml of water. The crystalline product is filtered off under suction, washed with a little water and dried. 78 g of 2,3-dichloro-4-trifluoromethyl-phenylhydrazine having a melting point of 79° to 80° C. are obtained.

後処理

  1. temperaturethe mixture is then heated to the reflux temperture for 12 hours
  2. distillationThereafter, 90% of the pyridine is distilled off
  3. filtrationThe crystalline product is filtered off under suction
  4. washwashed with a little water
  5. customdried

出典と根拠

ORDレコード
ord-84e111d02c504196864cc1b3e0ea59c4
出典データセット
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04764202

反応ノート

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