Trifluoroacetic acid → {6-Fluoro-5-[2-methyl-4-(2,3,4,5-tetrahydrobenzo[b]azepine-1-carbonyl)benzylcarbamoyl]-2-oxo-2,3,4,5-tetrahydrobenzo[b][1,4]diazepin-1-yl}-acetic acid

HRID 558951Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 558951
C([O:5][C:6](=[O:45])[CH2:7][N:8]1[C:14](=[O:15])[CH2:13][CH2:12][N:11]([C:16](=[O:39])[NH:17][CH2:18][C:19]2[CH:24]=[CH:23][C:22]([C:25]([N:27]3[CH2:33][CH2:32][CH2:31][CH2:30][C:29]4[CH:34]=[CH:35][CH:36]=[CH:37][C:28]3=4)=[O:26])=[CH:21][C:20]=2[CH3:38])[C:10]2[C:40]([F:44])=[CH:41][CH:42]=[CH:43][C:9]1=2)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[F:44][C:40]1[C:10]2[N:11]([C:16](=[O:39])[NH:17][CH2:18][C:19]3[CH:24]=[CH:23][C:22]([C:25]([N:27]4[CH2:33][CH2:32][CH2:31][CH2:30][C:29]5[CH:34]=[CH:35][CH:36]=[CH:37][C:28]4=5)=[O:26])=[CH:21][C:20]=3[CH3:38])[CH2:12][CH2:13][C:14](=[O:15])[N:8]([CH2:7][C:6]([OH:45])=[O:5])[C:9]=2[CH:43]=[CH:42][CH:41]=1

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 59807185{6-Fluoro-5-[2-methyl-4-(2,3,4,5-tetrahydrobenzo[b]azepine-1-carbonyl)-benzylcarbamoyl]-2-oxo-2,3,4,5-tetrahydrobenzo[b][1,4]diazepin-1-yl}acetic Acid Tert-Butyl Ester

Produkt 1

HCID 11699686{6-Fluoro-5-[2-methyl-4-(2,3,4,5-tetrahydrobenzo[b]azepine-1-carbonyl)benzylcarbamoyl]-2-oxo-2,3,4,5-tetrahydrobenzo[b][1,4]diazepin-1-yl}-acetic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of {6-fluoro-5-[2-methyl-4-(2,3,4,5-tetrahydrobenzo[b]azepine-1-carbonyl)benzylcabamoyl]-2-oxo-2,3,4,5-tetrahydrobenzo[b][1,4]diazepin-1-yl]acetic acid tert-butyl ester from Example 1 (250 mg, 0.40 mmol) in dichloromethane (8 ml) was added trifluoroacetic acid (8 ml). The mixture was stirred for 90 min and evaporated in vacuo and azeotroped with toluene to give an off-white solid; yield 220 mg, 99%.

Aufarbeitung

  1. customevaporated in vacuo
  2. customazeotroped with toluene
  3. customto give an off-white solid

Quellen und Nachweise

ORD-Eintrag
ord-18573718bc5d4498920c438613b81368
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08063038B2

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