Hydrazine hydrate (1:1) → 3-Chloro-2-hydrazinyl-5-(trifluoromethyl)pyridine

HRID 1266917ノート

反応式

HRID 1266917 の反応式
Cl[C:2]1[C:7]([Cl:8])=[CH:6][C:5]([C:9]([F:12])([F:11])[F:10])=[CH:4][N:3]=1.O.[NH2:14][NH2:15]>C(O)C>[Cl:8][C:7]1[C:2]([NH:14][NH2:15])=[N:3][CH:4]=[C:5]([C:9]([F:12])([F:11])[F:10])[CH:6]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 1122342,3-Dichloro-5-(trifluoromethyl)pyridine

生成物 1

HCID 12726913-Chloro-2-hydrazinyl-5-(trifluoromethyl)pyridine収率 70.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A reaction flask was loaded with 2,3-dichloro-5-(trifluoromethyl)pyridine (10.8 g) and ethanol (25 ml), followed by dropwise addition of hydrazine monohydrate (3 g) to the flask in 5 minutes with stirring. The resultant mixture was heated and stirred at 40 to 60° C. for 2.5 hours. Thereafter, the heating was stopped, and the reaction mixture was left to cool. The precipitated white crystals were filtrated for collection and dried to give 3-chloro-2-hydrazino-5-(trifluoromethyl)-pyridine (7.5 g).

後処理

  1. stirringstirred at 40 to 60° C. for 2.5 hours
  2. waitthe reaction mixture was left
  3. temperatureto cool
  4. filtrationThe precipitated white crystals were filtrated for collection
  5. customdried

出典と根拠

ORDレコード
ord-8b88ad2b25624016ac4929880adb8f1e
出典データセット
uspto-grants-2003_04
特許番号
US06551682B1

反応ノート

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