Reaktion #805753

ord-44756b00f1f54f2c985b360c3013a4ee

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was cooled
  2. 2
    FiltrationThe precipitated solid was collected by filtration
  3. 3
    Waschenwashed with MeOH (2×5 mL)
  4. 4
    Sonstigedried under high vacuum

Vorschrift

To a mixture of compound 5f (0.68 g, 1.7 mmol) and 2-methylquinoline (0.26 mL, 2.0 mmol) in DMF (5 mL) was added chlorotrimethylsilane (0.64 mL, 5.0 mmol) dropwise. The resulting mixture was stirred at 90° C. for 2 h. The reaction mixture was cooled, and water (20 mL) was added. The precipitated solid was collected by filtration, washed with MeOH (2×5 mL), and dried under high vacuum. Compound 5g was obtained as an orange solid. Mass Spectrum (LCMS, ESI pos.): Calcd. for C32H31 N5O3: 534.2 (M+H). found: 534.4.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09193736B2uspto-grants-2015_11