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Benzamidine → HCID 136454423, 화합물

HRID 1747788
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HRID 1747788 반응식
O=[C:2]([C:9]1[N:13]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:12]=[CH:11][CH:10]=1)[CH2:3][C:4]([O:6]CC)=O.[C:20]1([C:26](=[NH:28])[NH2:27])[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>CN(C=O)C>[C:20]1([C:26]2[NH:28][C:4](=[O:6])[CH:3]=[C:2]([C:9]3[N:13]([C:14]4[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=4)[N:12]=[CH:11][CH:10]=3)[N:27]=2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 2332BenzamidineHCID 89586101HCID 89586101, 화합물

생성물 1

HCID 136454423HCID 136454423, 화합물수율 27.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of ethyl 3-oxo-3-(1-phenyl-1H-pyrazol-5-yl)propanoate (300 mg) in DMF (10.0 mL) was added benzenecarboximidamide (139 mg) at room temperature. The reaction mixture was heated using a microwave reactor at 140° C. for 30 min. The reaction mixture was extracted with dichloromethane. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (dichloromethane/methanol) to give the title compound (100 mg).

후처리

  1. temperatureThe reaction mixture was heated
  2. customat 140° C.
  3. customfor 30 min
  4. extractionThe reaction mixture was extracted with dichloromethane
  5. washThe extract was washed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (dichloromethane/methanol)

출처 및 근거

ORD 기록
ord-3c67aabb5f6747748a2e79b054b882cb
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09150588B2

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