Ammonium Chloride → 3-(4-Cyclopropyl-piperazin-1-yl)-6-(3-nitro-phenyl)-pyridazine

HRID 80931

反応式

HRID 80931 の反応式
Cl[C:2]1[N:3]=[N:4][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([N+:14]([O-:16])=[O:15])[CH:9]=2)=[CH:6][CH:7]=1.[CH:17]1([N:20]2[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)[CH2:19][CH2:18]1.[NH4+].[Cl-]>CCCCO>[CH:17]1([N:20]2[CH2:25][CH2:24][N:23]([C:2]3[N:3]=[N:4][C:5]([C:8]4[CH:13]=[CH:12][CH:11]=[C:10]([N+:14]([O-:16])=[O:15])[CH:9]=4)=[CH:6][CH:7]=3)[CH2:22][CH2:21]2)[CH2:19][CH2:18]1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 47420041-CyclopropylpiperazineHCID 122575043-Chloro-6-(3-nitrophenyl)pyridazine

生成物 1

HCID 580066013-(4-Cyclopropyl-piperazin-1-yl)-6-(3-nitro-phenyl)-pyridazine収率 5.2%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
80 °C

実験手順

To a solution of 3-chloro-6-(3-nitro-phenyl)-pyridazine (10.0 g, 424 mmol) in n-BuOH (150 mL) was added 1-cyclopropyl-piperazine (8.55 g, 678 mmol) and NH4Cl (2.27 g, 424 mmol) and the mixture was stirred for 48 h at 80° C. The solvent was removed under reduced pressure, and the residue was diluted with water. After alkalization with ammonia, the mixture was extracted with ethyl acetate. The extract was dried (Na2SO4) and concentrated to give 7.2 g of crude 3-(4-cyclopropyl-piperazin-1-yl)-6-(3-nitro-phenyl)-pyridazine.

後処理

  1. customThe solvent was removed under reduced pressure
  2. additionthe residue was diluted with water
  3. extractionAfter alkalization with ammonia, the mixture was extracted with ethyl acetate
  4. dry with materialThe extract was dried (Na2SO4)
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-3666725acd2842338bbe8900b1198449
出典データセット
uspto-grants-2014_09
特許番号
US08846677B2

関連ノート

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