O-(Trimethylsilyl)hydroxylamine → HCID 178474861, Verbindung

HRID 351881

Reaktionsgleichung

Reaktionsgleichung von HRID 351881
C[Si](C)(C)[O:3][NH2:4].[C:7]([NH:10][CH2:11][C@@H:12]1[O:16][C:15](=[O:17])[N:14]([C:18]2[CH:23]=[CH:22][C:21]([C:24]#[N:25])=[C:20]([F:26])[CH:19]=2)[CH2:13]1)(=[O:9])[CH3:8]>C(O)C>[C:7]([NH:10][CH2:11][C@@H:12]1[O:16][C:15](=[O:17])[N:14]([C:18]2[CH:23]=[CH:22][C:21]([C:24](=[NH:25])[NH:4][OH:3])=[C:20]([F:26])[CH:19]=2)[CH2:13]1)(=[O:9])[CH3:8]

Komponenten

4

Edukt 2

HCID 2734666O-(Trimethylsilyl)hydroxylamineHCID 229661895-(S)-acetamidomethyl-3-[4'-cyano-3'-fluorophenyl]oxazolidine-2-one

Produkt 1

HCID 178474861HCID 178474861, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

O-Trimethylsilylhydroxylamine (0.37 ml, 3.0 mmol) and 5-(S)-acetamidomethyl-3-[4′-cyano-3′-fluorophenyl]oxazolidine-2-one (0.277 g, 1.0 mmol) in ethanol (3.0 ml) were stirred at 80° C. in a sealed reaction vial for 2.5 h. The mixture was left at r.t. for 48 h, and the crystallized product filtered, rinsed with ethanol (ca. 0.75 ml), washed with ether, and dried under vacuum. Yellow crystals. Yield 0.260 g (84%). HPLC: Rt 2.6 min. MS (m/z): [M+H]+=311.

Aufarbeitung

  1. filtrationthe crystallized product filtered
  2. washrinsed with ethanol (ca. 0.75 ml)
  3. washwashed with ether
  4. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-340c4767b10a46debfb353ea1607ee36
Quelldatensatz
uspto-grants-2004_06
Patentnummer
US06743811B2

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