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Benzamidine, hydrochloride → HCID 57839057, 화합물

HRID 732950
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HRID 732950 반응식
[Cl:1][C:2]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:3]=1[CH:4]=[C:5]([C:10](=O)[CH3:11])[C:6]([O:8][CH3:9])=[O:7].Cl.[C:19]([NH2:27])(=[NH:26])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.CC([O-])=O.[Na+]>CN(C=O)C>[Cl:1][C:2]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:3]=1[CH:4]1[C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:10]([CH3:11])[NH:27][C:19]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[N:26]1
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참가 물질

5

반응물 3

HCID 80289Benzamidine, hydrochlorideHCID 517045Sodium AcetateHCID 54009516Methyl 2-[(2,4-dichlorophenyl)methylidene]-3-oxobutanoate

생성물 1

HCID 57839057HCID 57839057, 화합물수율 88.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

To a stirred solution of methyl 2-(2,4-dichlorobenzylidene)-3-oxobutanoate (480 mg, 1.8 mmol) and benzamidine HCl salt (275 mg, 1.8 mmol) in DMF (6 mL) was added NaOAc (144 mg, 1.8 mmol). The reaction was heated to 60° C. for 3 days and was quenched by 1N HCl (10 mL). The reaction was diluted with EtOAc (10 mL) and the organic layer was washed with 1N HCl, saturated NH4Cl solution (10 mL) and brine (10 mL), dried (MgSO4), filtered and concentrated under reduced pressure to give the crude product as a yellow oil (600 mg). The crude reaction product was moved onto next step without further purification.

후처리

  1. customwas quenched by 1N HCl (10 mL)
  2. additionThe reaction was diluted with EtOAc (10 mL)
  3. washthe organic layer was washed with 1N HCl, saturated NH4Cl solution (10 mL) and brine (10 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-3c8afc35c77b4108b6915c84136cd3c3
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07589088B2

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