Trifluoroacetic acid → 2-Methyl-N-(5-methyl-6-oxo-6,7-dihydro-5H-dibenzo[b,d]azepin-7-yl)-malonamic acid

HRID 2223307Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2223307
C(O)(C(F)(F)F)=O.C([O:12][C:13](=[O:36])[CH:14]([CH3:35])[C:15]([NH:17][CH:18]1[C:24](=[O:25])[N:23]([CH3:26])[C:22]2[CH:27]=[CH:28][CH:29]=[CH:30][C:21]=2[C:20]2[CH:31]=[CH:32][CH:33]=[CH:34][C:19]1=2)=[O:16])(C)(C)C>ClCCl>[CH3:35][CH:14]([C:15]([NH:17][CH:18]1[C:24](=[O:25])[N:23]([CH3:26])[C:22]2[CH:27]=[CH:28][CH:29]=[CH:30][C:21]=2[C:20]2[CH:31]=[CH:32][CH:33]=[CH:34][C:19]1=2)=[O:16])[C:13]([OH:36])=[O:12]

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 690397662-methyl-N-(5-methyl-6-oxo-6,7-dihydro-5H-dibenzo[b,d]azepin-7-yl)-malonamic acid tert-butyl ester

Produkt 1

HCID 210725002-Methyl-N-(5-methyl-6-oxo-6,7-dihydro-5H-dibenzo[b,d]azepin-7-yl)-malonamic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

TFA (3 ml) was added to a solution of 2-methyl-N-(5-methyl-6-oxo-6,7-dihydro-5H-dibenzo[b,d]azepin-7-yl)-malonamic acid tert-butyl ester (920 mg, 2.33 mmol) in dichloromethane (3 ml) and the mixture was stirred at r.t. overnight. The mixture was then taken up in more dichloromethane, washed with water, and dried (Na2SO4). After evaporation of the solvent, the title compound, MS: m/e=339.3 (M+H+), (580 mg, 73%) was obtained by chromatographic purification of the residue (silica gel, MeOH, CH2Cl2).

Aufarbeitung

  1. washwashed with water
  2. dry with materialdried (Na2SO4)
  3. customAfter evaporation of the solvent

Quellen und Nachweise

ORD-Eintrag
ord-8c0d1e494a42468f99c0b8b07b9b1870
Quelldatensatz
uspto-grants-2008_05
Patentnummer
US07375099B2

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