Water → N-[4-(Pyrido[2,3-b][1,5]benzoxazepin-6(5H)-ylcarbonyl)-3-chlorophenyl][1,1'-biphenyl]-2-carboxamide

HRID 1457694

Reaktionsgleichung

Reaktionsgleichung von HRID 1457694
[N:1]1[C:6]2[O:7][C:8]3[CH:15]=[CH:14][CH:13]=[CH:12][C:9]=3[NH:10][CH2:11][C:5]=2[CH:4]=[CH:3][CH:2]=1.C(N(CC)C(C)C)(C)C.[C:25]1([C:44]2[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=2)[C:26]([C:31]([NH:33][C:34]2[CH:42]=[CH:41][C:37]([C:38](Cl)=[O:39])=[C:36]([Cl:43])[CH:35]=2)=[O:32])=[CH:27][CH:28]=[CH:29][CH:30]=1.O>ClCCl>[N:1]1[C:6]2[O:7][C:8]3[CH:15]=[CH:14][CH:13]=[CH:12][C:9]=3[N:10]([C:38]([C:37]3[CH:41]=[CH:42][C:34]([NH:33][C:31]([C:26]4[C:25]([C:44]5[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=5)=[CH:30][CH:29]=[CH:28][CH:27]=4)=[O:32])=[CH:35][C:36]=3[Cl:43])=[O:39])[CH2:11][C:5]=2[CH:4]=[CH:3][CH:2]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 158959295,6-Dihydropyrido[2,3-b][1,5]benzoxazepineHCID 220996004-[([1,1'-Biphenyl]-2-carbonyl)amino]-2-chlorobenzoyl chloride

Produkt 1

HCID 22099925N-[4-(Pyrido[2,3-b][1,5]benzoxazepin-6(5H)-ylcarbonyl)-3-chlorophenyl][1,1'-biphenyl]-2-carboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 0.198 g of 5,6-dihydropyrido[2,3-b][1,5]benzoxazepine, 0.155 g of N,N-diisopropylethylamine and 0.444 g of 4-[([1,1-biphenyl]-2-carbonyl)amino]-2-chlorobenzoyl chloride in 12 ml of dichloromethane is stirred at room temperature for 2.5 hours. The mixture is poured into water and extracted with dichloromethane. The extract is washed with 2N Na2CO3, H2O, brine and dried (Na2 SO4). The solution is passed through a thin pad of hydrous magnesium silicate. The filter pad is washed with 50 ml of hexane-ethyl acetate (1:2) and the filtrate concentrated to dryness.

Aufarbeitung

  1. extractionextracted with dichloromethane
  2. washThe extract is washed with 2N Na2CO3, H2O, brine
  3. customdried (Na2 SO4)
  4. washThe filter pad is washed with 50 ml of hexane-ethyl acetate (1:2)
  5. concentrationthe filtrate concentrated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-fe7620382d5a4248a662034564e8e059
Quelldatensatz
uspto-grants-1998_12
Patentnummer
US05849735

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