Reaktion #1345023

ord-018cfa94993f48388c9742b39d74a472

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe ice-water bath was removed
  2. 2
    Waschenwashed with water, and brine
  3. 3
    TrocknenThe organic layer was dried over Na2SO4
  4. 4
    Filtrationfiltered
  5. 5
    Einengenconcentrated under reduced pressure
  6. 6
    SonstigeThe residue (220 mg, 83.9%) was directly used in next step without further purification

Vorschrift

Methyl chloroformate (85.0 μL, 1.1 mmol) was added to a solution of 1-(4-bromo-2-fluorophenyl)methanamine (0.204 g, 1.0 mmol) and triethylamine (148.1 μL, 1.1 mmol) in methylene chloride (5 mL) at 0° C. After 10 min, the ice-water bath was removed. The mixture was stirred at RT for 1 h, washed with water, and brine. The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue (220 mg, 83.9%) was directly used in next step without further purification. LCMS: (M+H)=263.9/261.8.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08461330B2uspto-grants-2013_06