1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 10385550, 화합물

HRID 1242885노트

반응식

HRID 1242885 반응식
CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.[CH3:22][N:23]([CH3:27])[CH2:24][CH2:25][NH2:26].[C:28]1([C:46]2[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=2)[CH:33]=[CH:32][C:31]([C:34]([NH:36][C:37]2[CH:45]=[CH:44][C:40]([C:41]([O-])=[O:42])=[CH:39][CH:38]=2)=[O:35])=[CH:30][CH:29]=1>C1COCC1.C(#N)C.C(OCC)(=O)C.O.C(N(CC)CC)C>[CH3:22][N:23]([CH3:27])[CH2:24][CH2:25][NH:26][C:41]([C:40]1[CH:39]=[CH:38][C:37]([NH:36][C:34]([C:31]2[CH:32]=[CH:33][C:28]([C:46]3[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=3)=[CH:29][CH:30]=2)=[O:35])=[CH:45][CH:44]=1)=[O:42]

참가 물질

10

반응물 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 66053N,N-DimethylethylenediamineHCID 757711-HydroxybenzotriazoleHCID 7040114HCID 7040114, 화합물

생성물 1

HCID 10385550HCID 10385550, 화합물수율 25.3%

시약·촉매·용매 5

HCID 962Water용매HCID 6342Acetonitrile용매HCID 8028Tetrahydrofuran용매HCID 8471Triethylamine용매HCID 8857Ethyl Acetate용매

실험 절차

WSC (0.248 g), HOBt (0.156 g), N,N-dimethyl ethylenediamine (0.097 g) and triethylamine (0.21 ml) were added to a mixed solution of 4-(4-biphenylylcarbonylamino)benzoate (0.323 g) in THF (15 ml) and acetonitrile (15 ml). After stirring at room temperature for 18 hours, water was added to the reaction mixture, and extraction was conducted using ethyl acetate. The organic layer was washed with 10% aqueous potassium carbonate and saturated aqueous sodium chloride solution, dried, and then concentrated. The residue was recrystallized using methanol/diethyl ether to give the titled compound (0.100 g).

후처리

  1. washThe organic layer was washed with 10% aqueous potassium carbonate and saturated aqueous sodium chloride solution
  2. customdried
  3. concentrationconcentrated
  4. customThe residue was recrystallized

출처 및 근거

ORD 기록
ord-fc5eddb1212c45ee9373ad34bd861204
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07115750B1

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