Hydrazine hydrate (1:1) → 4-(4-Chlorophenyl)-2-hydrazinyl-3,4'-bipyridine

HRID 2101316

反応式

HRID 2101316 の反応式
Cl[C:2]1[C:7]([C:8]2[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=2)=[C:6]([C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)[CH:5]=[CH:4][N:3]=1.O.[NH2:22][NH2:23]>N1C=CC=CC=1>[Cl:20][C:17]1[CH:18]=[CH:19][C:14]([C:6]2[CH:5]=[CH:4][N:3]=[C:2]([NH:22][NH2:23])[C:7]=2[C:8]2[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=2)=[CH:15][CH:16]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 577993632-Chloro-4-(4-chlorophenyl)-3,4'-bipyridine

生成物 1

HCID 577994604-(4-Chlorophenyl)-2-hydrazinyl-3,4'-bipyridine収率 78.4%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a stirring solution of 2-chloro-4-(4-chlorophenyl)-3,4′-bipyridine (1.3 g, 4.3 mmol) in pyridine (5 mL) at room temperature under argon was added hydrazine monohydrate (2.5 mL, 51.5 mmol). The reaction mixture was stirred at reflux under argon for 15 h. After cooling the reaction mixture to room temperature, most of the solvent was removed under reduced pressure. Water (25 mL) was added to the residue while stirring and a precipitate formed. The precipitate was collected by filtration and washed with water (15 mL×2). After drying under reduced pressure at elevated temperature, 1.0 g of the title compound was obtained as a yellow solid. HPLC/MS: retention time=1.68 min, [M+H]+=297.

後処理

  1. temperatureat reflux under argon for 15 h
  2. custommost of the solvent was removed under reduced pressure
  3. additionWater (25 mL) was added to the residue
  4. stirringwhile stirring
  5. customa precipitate formed
  6. filtrationThe precipitate was collected by filtration
  7. washwashed with water (15 mL×2)
  8. customAfter drying under reduced pressure at elevated temperature

出典と根拠

ORDレコード
ord-9ee2c7577d5a455c859b9b5cbe713725
出典データセット
uspto-grants-2009_08
特許番号
US07572808B2

関連ノート

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