Reaktion #422254

ord-014c893496e74cd29bc729cfbd079aa3

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with CH2Cl2
  2. 2
    TrocknenThe organic layer was dried with sodium sulfate
  3. 3
    Filtrationfiltered
  4. 4
    Einengenconcentrated

Vorschrift

A 250 mL round-bottomed flask was charged with 5-chloropyridin-2-amine (80 g, 622.3 mmol) and CHCl3 (100 mL). Added bromine (31.98 mL, 622.3 mmol) and stirred at room temperature for 30 minutes. The reaction mixture was poured into saturated bicarbonate and NaHSO3 and extracted with CH2Cl2. The organic layer was dried with sodium sulfate, filtered and concentrated to afford the title compound (113.8 g, 88.1% yield) as a tan solid. 1H NMR (d6-DMSO) δ 7.97 (d, 1H), 7.90 (d, 1H), 6.44 (bs, 2H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08883828B2uspto-grants-2014_11