3-Methoxybenzylamine → HCID 57754052, Verbindung

HRID 226213

Reaktionsgleichung

Reaktionsgleichung von HRID 226213
[C:1]([O:5][C:6](=[O:21])[NH:7][C@@H:8]([C@H:18]1[CH2:20][O:19]1)[CH2:9][C:10]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]([F:17])[CH:11]=1)([CH3:4])([CH3:3])[CH3:2].[O-]S(C(F)(F)F)(=O)=O.[Li+].[CH3:31][O:32][C:33]1[CH:34]=[C:35]([CH:38]=[CH:39][CH:40]=1)[CH2:36][NH2:37].[Cl-].[NH4+]>C(#N)C>[C:1]([O:5][C:6](=[O:21])[NH:7][C@@H:8]([CH2:9][C:10]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]([F:17])[CH:11]=1)[C@H:18]([OH:19])[CH2:20][NH:37][CH2:36][C:35]1[CH:38]=[CH:39][CH:40]=[C:33]([O:32][CH3:31])[CH:34]=1)([CH3:4])([CH3:3])[CH3:2]

Komponenten

6

Edukt 4

HCID 211563-MethoxybenzylamineHCID 25517Ammonium ChlorideHCID 3664839Trifluoromethanesulfonic acid, lithium saltHCID 86616462(1R,2S)-[2-(3,4-difluoro-phenyl)-1-oxiranyl-ethyl]-carbamic acid tert-butyl ester

Produkt 1

HCID 57754052HCID 57754052, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A solution of (1R,2S)-[2-(3,4-difluoro-phenyl)-1-oxiranyl-ethyl]-carbamic acid tert-butyl ester (0.03 g, 0.1 mmol) in acetonitrile (1 mL) was treated with lithium triflate (0.032 g, 0.2 mmol) and stirred at ambient temperature for 20 minutes. Then 3-methoxybenzylamine (0.016 mL, 0.12 mmol) was added to the reaction neat in one portion. The reaction was stirred at ambient temperature for 14 hours. The reaction was poured into saturated ammonium chloride solution (5 mL), extracted with ethyl acetate, the organic phase separated, dried (MgSO4) and the solvent removed at reduced pressure. The product was obtained as an oil and used without further purification (0.041 g, 94%). MS: 437 (M+H, 100%).

Aufarbeitung

  1. stirringThe reaction was stirred at ambient temperature for 14 hours
  2. extractionextracted with ethyl acetate
  3. customthe organic phase separated
  4. dry with materialdried (MgSO4)
  5. customthe solvent removed at reduced pressure
  6. customThe product was obtained as an oil
  7. customused without further purification (0.041 g, 94%)

Quellen und Nachweise

ORD-Eintrag
ord-102b0fd138274c048ebe5de232edecef
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07557137B2

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