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1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → HCID 67960127, 화합물

HRID 1529366
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HRID 1529366 반응식
[C:1]([O:5][C:6]([N:8]1[C:16]2[C:11](=[CH:12][C:13]([C:17](O)=[O:18])=[CH:14][CH:15]=2)[C:10]([I:20])=[CH:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].CC[N:23]=C=NCCCN(C)C.Cl>CN(C=O)C>[C:17]([C:13]1[CH:12]=[C:11]2[C:16](=[CH:15][CH:14]=1)[N:8]([C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7])[CH:9]=[C:10]2[I:20])(=[O:18])[NH2:23]
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참가 물질

4

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HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 67958597HCID 67958597, 화합물

생성물 1

HCID 67960127HCID 67960127, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To solution of 1-(tert-butoxycarbonyl)-3-iodo-1H-indole-5-carboxylic acid (1 g, 2.57 mmol) in DMF (10 mL) at 0° C. was added EDC.HCl (741 mg, 3.86 mmol) and HOBT-NH3 complex (825 mg, 5.15 mmol). The reaction mixture was stirred at RT for 3 h and then extracted with DCM (15 mL). The organic layer was washed with brine, dried over Na2SO4, filtered, and concentrated to dryness. The crude product was purified by column chromatography to obtain title compound as an off white solid (550 mg, 50%). MS (ESI, Neg. ion) m/z: 286.9 (M+1).

후처리

  1. extractionextracted with DCM (15 mL)
  2. washThe organic layer was washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated to dryness
  6. customThe crude product was purified by column chromatography

출처 및 근거

ORD 기록
ord-3083beb5bd8f4233858dadc8edc48182
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09090593B2

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