Reaktion #51616

ord-60dc820a1ebd4013beebac37a1fde919

Reaktionsbedingungen

Temperatur
135°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe mix is partitioned between CH2Cl2 and saturated NaHCO3
  2. 2
    TrocknenThe organic layer is dried (MgSO4)
  3. 3
    Einengenconcentrated
  4. 4
    SonstigeThe resulting syrup is chromatographed (1:1 EtOAc:CH2Cl2)

Vorschrift

To 0.3 g (1.34 mmol) of 2-chloro-6,7-dimethoxyquinoxaline is added approx. 1 mL of cyclohexylamine. The mixture is heated overnight at 105° C. and a further 10 hours at 135° C. The mix is partitioned between CH2Cl2 and saturated NaHCO3. The organic layer is dried (MgSO4) and concentrated. The resulting syrup is chromatographed (1:1 EtOAc:CH2Cl2) to provide 0.265 g of the product as a lt. brown solid in 69% yield (m.p. 188-189.5). Anal. calcd for C16H21N3O2: C, 66.88; H, 7.37; N, 14.62. Found: C, 66.82; H, 7.28; N, 14.45.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06852712B2uspto-grants-2005_02