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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 10411283, 화합물

HRID 1991088
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HRID 1991088 반응식
[C:1]([NH:4][C:5]1[CH:10]=[C:9]([Cl:11])[CH:8]=[CH:7][C:6]=1/[CH:12]=[CH:13]/[C:14]([OH:16])=O)(=[O:3])[CH3:2].[Cl:17][C:18]1[CH:31]=[CH:30][C:21]([CH2:22][N:23]2[CH2:28][CH2:27][NH:26][CH:25]([CH3:29])[CH2:24]2)=[CH:20][CH:19]=1.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C>[Cl:11][C:9]1[CH:8]=[CH:7][C:6](/[CH:12]=[CH:13]/[C:14]([N:26]2[CH2:27][CH2:28][N:23]([CH2:22][C:21]3[CH:30]=[CH:31][C:18]([Cl:17])=[CH:19][CH:20]=3)[CH2:24][CH:25]2[CH3:29])=[O:16])=[C:5]([NH:4][C:1](=[O:3])[CH3:2])[CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 60137954HCID 60137954, 화합물HCID 68538268HCID 68538268, 화합물

생성물 1

HCID 10411283HCID 10411283, 화합물수율 63.2%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

0.10 g (0.42 mmol) (E)-3-(2-Acetylamino-4-chloro-phenyl)-acrylic acid, 85 mg 1-(4-Chloro-benzyl)-3-methyl-piperazine (0.38 mmol), 87 mg EDCI (0.45 mmol) and 61 mg HOBt (0.45 mmol) were dissolved in 5 ml DMF. The reaction mixture was stirred overnight, then partitioned between ethylacetate and aq. sodiumbicarbonate solution. The organic phase was further washed with water and brine. Removal of the solvent gave a crude product which was further purified by prep. HPLC (Waters XT column, acetonitrile/water). 0.11 mg (0.24 mmol, 63%) of the title compound was obtained as an pale yellow solid.

후처리

  1. custompartitioned between ethylacetate and aq. sodiumbicarbonate solution
  2. washThe organic phase was further washed with water and brine
  3. customRemoval of the solvent
  4. customgave a crude product which
  5. customwas further purified by prep

출처 및 근거

ORD 기록
ord-7c5f9089110a4b3ba91cc674a4fbdaf3
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07645760B2

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