Trimethylamine → (2-{7-chloro-1-[2-methyl-4-(2-methyl-benzoylamino)-benzoyl]-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yloxycarbonylamino}-ethyl)-trimethyl-ammonium chloride

HRID 1184655Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1184655
[CH3:1][N:2]([CH3:4])[CH3:3].[Cl:5][C:6]1[CH:42]=[CH:41][C:9]2[N:10]([C:22](=[O:40])[C:23]3[CH:28]=[CH:27][C:26]([NH:29][C:30](=[O:38])[C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=4[CH3:37])=[CH:25][C:24]=3[CH3:39])[CH2:11][CH2:12][CH2:13][CH:14]([O:15][C:16](=[O:21])[NH:17][CH2:18][CH2:19]Cl)[C:8]=2[CH:7]=1>C(O)C>[Cl-:5].[Cl:5][C:6]1[CH:42]=[CH:41][C:9]2[N:10]([C:22](=[O:40])[C:23]3[CH:28]=[CH:27][C:26]([NH:29][C:30](=[O:38])[C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=4[CH3:37])=[CH:25][C:24]=3[CH3:39])[CH2:11][CH2:12][CH2:13][CH:14]([O:15][C:16]([NH:17][CH2:18][CH2:19][N+:2]([CH3:4])([CH3:3])[CH3:1])=[O:21])[C:8]=2[CH:7]=1

Komponenten

4

Edukt 2

HCID 1146TrimethylamineHCID 86708937{7-chloro-1-[2-methyl-4-(2-methyl-benzoylamino)-benzoyl]-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl} (2-chloroethyl)carbamate

Produkt 1

HCID 66733336(2-{7-chloro-1-[2-methyl-4-(2-methyl-benzoylamino)-benzoyl]-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yloxycarbonylamino}-ethyl)-trimethyl-ammonium chloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
170 °C

Versuchsvorschrift

Trimethylamine (30% solution, 0.5 ml) was added to an ethanol solution (10 ml) of {7-chloro-1-[2-methyl-4-(2-methyl-benzoylamino)-benzoyl]-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl}(2-chloroethy)carbamate (330 mg), and the mixture was heated at 170° C. for 15 minutes (microwave reactor). After cooling to room temperature, the reaction mixture was concentrated under reduced pressure. To the residue was added ethyl acetate, and the resulted precipitates were collected by filtration and dried to obtain 120 mg of (2-{7-chloro-1-[2-methyl-4-(2-methyl-benzoylamino)-benzoyl]-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yloxycarbonylamino}-ethyl)-trimethyl-ammonium chloride as white powder.

Aufarbeitung

  1. temperatureAfter cooling to room temperature
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. additionTo the residue was added ethyl acetate
  4. customthe resulted precipitates
  5. filtrationwere collected by filtration
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-6c0d5483d93848f9b239894fa64db28b
Quelldatensatz
uspto-grants-2014_03
Patentnummer
US08669229B2

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