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

HRID 1356474노트

반응식

HRID 1356474 반응식
[C:1]1([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:6]=[CH:5][C:4]([C:7]([NH:9][C:10]2[CH:18]=[CH:17][C:13]([C:14](O)=[O:15])=[CH:12][CH:11]=2)=[O:8])=[CH:3][CH:2]=1.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.[CH3:46][N:47]([CH3:51])[CH2:48][CH2:49][NH2:50]>C1COCC1.O.C(N(CC)CC)C.C(#N)C>[CH3:46][N:47]([CH3:51])[CH2:48][CH2:49][NH:50][C:14]([C:13]1[CH:12]=[CH:11][C:10]([NH:9][C:7]([C:4]2[CH:5]=[CH:6][C:1]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[CH:2][CH:3]=2)=[O:8])=[CH:18][CH:17]=1)=[O:15]

참가 물질

9

반응물 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 66053N,N-DimethylethylenediamineHCID 757711-HydroxybenzotriazoleHCID 4590482HCID 4590482, 화합물

생성물 1

HCID 10385550HCID 10385550, 화합물수율 25.4%

시약·촉매·용매 4

HCID 962Water용매HCID 6342Acetonitrile용매HCID 8028Tetrahydrofuran용매HCID 8471Triethylamine용매

실험 절차

To a solution of 4-(4-biphenylylcarbonylamino)benzoic acid (0.323 g) in THF (15 ml)/acetonitrile (15 ml) were added WSC (0.248 g), HOBt (0.156 g), N,N-dimethylethylenediamine (0.097 g), and triethylamine (0.21 ml). After stirring at room temperature for 18 hr, the reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with 10% aqueous potassium carbonate and saturated aqueous sodium chloride sequentially, dried, and concentrated. The residue was recrystallized from methanol/diethyl ether to obtain the titled compound (0.100 g).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with 10% aqueous potassium carbonate and saturated aqueous sodium chloride sequentially
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was recrystallized from methanol/diethyl ether

출처 및 근거

ORD 기록
ord-f992392759f9421c9254a34c15317e6e
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06586475B1

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