Cyclopentylhydrazine hydrochloride → HCID 86694313, 화합물

HRID 69109

반응식

HRID 69109 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[CH2:9][C:10](=O)[CH3:11])=[C:4]([N+:14]([O-:16])=[O:15])[CH:3]=1.Cl.[CH:18]1([NH:23][NH2:24])[CH2:22][CH2:21][CH2:20][CH2:19]1>C(O)(=O)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:23]([CH:18]3[CH2:22][CH2:21][CH2:20][CH2:19]3)[N:24]=[C:10]([CH3:11])[CH:9]=2)=[C:4]([N+:14]([O-:16])=[O:15])[CH:3]=1

참가 물질

4

반응물 2

HCID 212349Cyclopentylhydrazine hydrochlorideHCID 866943141-(4-Bromo-2-nitrophenyl)butane-1,3-dione

생성물 1

HCID 86694313HCID 86694313, 화합물수율 62.9%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
100 °C

실험 절차

Under a nitrogen atmosphere, to a solution of 1.0 g of 1-(4-bromo-2-nitrophenyl)butane-1,3-dione in 10 ml of acetic acid was added 501 mg of cyclopentylhydrazine hydrochloride, followed by stirring at 100° C. for 1 hour and 30 minutes. The reaction mixture was concentrated, and to the obtained residue was added ethyl acetate. The solution was washed with a saturated aqueous sodium hydrogen carbonate solution and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and then the residue was purified by silica gel column chromatography (chloroform/methanol) to obtain 770 mg of 5-(4-bromo-2-nitrophenyl)-1-cyclopentyl-3-methyl-1H-pyrazole.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. additionto the obtained residue was added ethyl acetate
  3. washThe solution was washed with a saturated aqueous sodium hydrogen carbonate solution and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (chloroform/methanol)

출처 및 근거

ORD 기록
ord-a380d65bfdde4e3f8411965e030bc974
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822448B2

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