Sodium Carbonate → 6-methoxy-2-methyl-3-[(3S,9aR)-octahydropyrazino[2,1-c][1,4]oxazin-3-yl]benzonitrile

HRID 2175897Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2175897
FC(F)(F)[C:3](O)=[O:4].F[C:9]1[C:14]([C:15]#[N:16])=[C:13]([CH3:17])[C:12]([C@@H:18]2[O:23][CH2:22][C@H:21]3[CH2:24][NH:25][CH2:26][CH2:27][N:20]3[CH2:19]2)=[CH:11][CH:10]=1.C(=O)([O-])[O-].[Na+].[Na+]>CO>[CH3:3][O:4][C:9]1[C:14]([C:15]#[N:16])=[C:13]([CH3:17])[C:12]([C@@H:18]2[O:23][CH2:22][C@H:21]3[CH2:24][NH:25][CH2:26][CH2:27][N:20]3[CH2:19]2)=[CH:11][CH:10]=1

Komponenten

4

Edukt 2

HCID 10340Sodium CarbonateHCID 867270976-fluoro-2-methyl-3-[(3S,9aR)-octahydropyrazino[2,1-c][1,4]oxazin-3-yl]benzonitrile trifluoroacetate

Produkt 1

HCID 867270966-methoxy-2-methyl-3-[(3S,9aR)-octahydropyrazino[2,1-c][1,4]oxazin-3-yl]benzonitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

A microwave vial was charged with 6-fluoro-2-methyl-3-[(3S,9aR)-octahydropyrazino[2,1-c][1,4]oxazin-3-yl]benzonitrile trifluoroacetate (110 mg, 0.290 mmol), sodium carbonate (30 mg, 0.290 mmol), and methanol (2 mL). The mixture was heated to 150° C. in a microwave apparatus for 2 h, then cooled to ambient temperature, filtered and concentrated to provide the title compound which was used without further purification. LC-MS (IE, m/z): 288 [M+1]+.

Aufarbeitung

  1. temperaturecooled to ambient temperature
  2. filtrationfiltered
  3. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-0845fe58979e4325bfa446a228a7f342
Quelldatensatz
uspto-grants-2015_06
Patentnummer
US09062070B2

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