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Isobutylamine → 10-[[6-[(2-Methylpropyl)amino]-3-pyridinyl]carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine

HRID 976413
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 976413
Cl[C:2]1[N:7]=[CH:6][C:5]([C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[CH2:14][N:13]3[CH:21]=[CH:22][CH:23]=[C:12]3[CH2:11]2)=[O:9])=[CH:4][CH:3]=1.[CH3:24][CH:25]([CH3:28])[CH2:26][NH2:27].CC1N(C(N(C)C)=O)C1>N1C=CC=CC=1>[CH3:24][CH:25]([CH3:28])[CH2:26][NH:27][C:2]1[N:7]=[CH:6][C:5]([C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[CH2:14][N:13]3[CH:21]=[CH:22][CH:23]=[C:12]3[CH2:11]2)=[O:9])=[CH:4][CH:3]=1
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Komponenten

5

Edukt 3

HCID 6558IsobutylamineHCID 11007919N,N,2-trimethylaziridine-1-carboxamideHCID 2194772510-[(6-Chloro-3-pyridinyl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine

Produkt 1

HCID 1891756210-[[6-[(2-Methylpropyl)amino]-3-pyridinyl]carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049
Pyridine
Lösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 0.16 g of 10-[(6-chloro-3-pyridinyl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 40 mg of pyridine and 2 ml of 2-methylpropylamine is stirred and heated at 100° C. in a sealed vessel for 1 hour. To the mixture is added 0.2 ml of N,N-dimethylpropyleneurea and the mixture is heated at 110° C. for 7 hours. The volatiles are removed under vacuum and 10 ml of 0.5N NaOH is added to the residue. The mixture is filtered and the solid washed with water and then hexane. The solid is dissolved in ethyl acetate and the solution washed with 0.5N NaOH, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrous magnesium silicate and the filtrate concentrated to dryness. The residue is triturated with diisopropylether-hexane to give 0.18 g of white solid; mass spectrum (CI) 361 (M+H).

Aufarbeitung

  1. temperaturethe mixture is heated at 110° C. for 7 hours
  2. customThe volatiles are removed under vacuum and 10 ml of 0.5N NaOH
  3. additionis added to the residue
  4. filtrationThe mixture is filtered
  5. washthe solid washed with water
  6. dissolutionThe solid is dissolved in ethyl acetate
  7. washthe solution washed with 0.5N NaOH, brine
  8. dry with materialdried (Na2SO4)
  9. filtrationThe solution is filtered through a thin pad of hydrous magnesium silicate
  10. concentrationthe filtrate concentrated to dryness
  11. customThe residue is triturated with diisopropylether-hexane

Quellen und Nachweise

ORD-Eintrag
ord-063459f5e9084ee0b506150d0b8beda2
Quelldatensatz
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05612334

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