Reaktion #74190

ord-22037d73702f4e76aa4d49714ff01bb4

Reagenzien

Keine

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted twice with ethyl ether
  2. 2
    Waschenwashed with water
  3. 3
    Trocknensaturated aqueous NaCl, dried over MgSO4
  4. 4
    Filtrationfiltered
  5. 5
    Einengenconcentrated

Vorschrift

D-Leucine (8.2 g, 62.7 mmol) was dissolved in 3.0M HBr in water (99 mL, 0.3 mol) and cooled to 0° C. A solution of NaNO2 (6.9 g, 100 mmol) in water (11.3 mL, 627 mmol) was slowly added over 20 minutes. The mixture was stirred at 0° C. for 3 hours and then extracted twice with ethyl ether, washed with water then saturated aqueous NaCl, dried over MgSO4, filtered, and concentrated to afford (R)-2-bromo-4-methylpentanoic acid (11.5 g) as an off-yellow oil. This was taken on to the next step without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08541597B2uspto-grants-2013_09