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Diisopropylethylamine → 3,5-dichloro-4-({4-[(cyclopropylcarbonyl)amino]-1H-pyrrolo[3,2-c]pyridin-1-yl}carbonyl)-N-ethylbenzamide

HRID 2201854
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HRID 2201854 반응식
[Cl:1][C:2]1[CH:10]=[C:9]([C:11](=[O:15])[NH:12][CH2:13][CH3:14])[CH:8]=[C:7]([Cl:16])[C:3]=1[C:4]([OH:6])=O.ON1C2N=CC=CC=2N=N1.C[NH3+].F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1.F[P-](F)(F)(F)(F)F.[NH:60]1[C:68]2[CH:67]=[CH:66][N:65]=[C:64]([NH:69][C:70]([CH:72]3[CH2:74][CH2:73]3)=[O:71])[C:63]=2[CH:62]=[CH:61]1.C(N(CC)C(C)C)(C)C>CN(C)C1C=CC=CC=1.O>[Cl:16][C:7]1[CH:8]=[C:9]([CH:10]=[C:2]([Cl:1])[C:3]=1[C:4]([N:60]1[C:68]2[CH:67]=[CH:66][N:65]=[C:64]([NH:69][C:70]([CH:72]3[CH2:73][CH2:74]3)=[O:71])[C:63]=2[CH:62]=[CH:61]1)=[O:6])[C:11]([NH:12][CH2:13][CH3:14])=[O:15]
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참가 물질

8

반응물 5

HCID 81531DiisopropylethylamineHCID 181649HOAtHCID 710615382,6-Dichloro-4-(ethylcarbamoyl)benzoic acidHCID 866211442-(1H-7-Azabenzotriazol-1-yl)-1,1,3,3-tetramethyl uronium hexafluorophosphate MethanaminiumHCID 86720627N-(1H-pyrrolo[3,2-c]pyridin-4-yl)cyclopropanecarboxamide

생성물 1

HCID 71618615
3,5-dichloro-4-({4-[(cyclopropylcarbonyl)amino]-1H-pyrrolo[3,2-c]pyridin-1-yl}carbonyl)-N-ethylbenzamide
수율 26.6%

시약·촉매·용매 2

HCID 949N,N-Dimethylaniline용매HCID 962Water용매

실험 절차

A well stirred mixture of 2,6-dichloro-4-(ethylcarbamoyl)benzoic acid (84.6 mg, 0.42 mmol), 1-hydroxy-7-azabenzotriazole (77 mg, 0.57 mmol), N,N-dimethyl aminopyridine (22 mg, 0.11 mmol) and 2-(1H-7-azabenzotriazol-1-yl)-1,1,3,3-tetramethyl uronium hexafluorophosphate methanaminium (216 mg, 0.57 mmol) in N,N-dimethylaniline was treated with N-(1H-pyrrolo[3,2-c]pyridin-4-yl)cyclopropanecarboxamide (100 mg, 0.38 mmol) and N,N-diisopropylethylamine (0.1 ml, 0.95 mmol). The reaction was stirred overnight at room temperature. The contents were diluted with water and extracted with ethyl acetate. The combined organic portion was washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated. The crude product was purified by silica gel column chromatography using methanol in dichloromethane (3%) as eluent to yield 3,5-dichloro-4-({4-[(cyclopropylcarbonyl)amino]-1H-pyrrolo[3,2-c]pyridin-1-yl}carbonyl)-N-ethylbenzamide (45 mg, 26%) as an off white solid.

후처리

  1. stirringThe reaction was stirred overnight at room temperature
  2. extractionextracted with ethyl acetate
  3. washThe combined organic portion was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude product was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-75cc998b079940d7bb1d04eed81dd4f6
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09364466B2

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