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

HRID 80931

반응식

HRID 80931 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 2631-Butanol용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3666725acd2842338bbe8900b1198449
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846677B2

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