Reaktion #86500

ord-98472b128ff34c7080db4dbfec015a2b

Reagenzien

Keine

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    Sonstigeat 0° C.
  2. 2
    Temperaturto warm to room temperature overnight
  3. 3
    workup.STIRRINGWhile stirring
  4. 4
    Sonstigea stream of air was bubbled through the solution for 1 hour
  5. 5
    TrocknenThe reaction mixture was dried over sodium sulfate
  6. 6
    Sonstigethe solvent evaporated under reduced pressure

Vorschrift

Under a nitrogen atmosphere, a solution of bromine (8.61 mL, 167 mmol) in chloroform (20 mL) was added drop-wise over a period of 2 h to a solution of methyl 3-oxohexanoate (Fluka, 24.1 g, 167 mmol) in chloroform (147 mL), at 0° C. (ice bath). The reaction mixture was stirred for 30 min at 0° C. and then allowed to warm to room temperature overnight. While stirring, a stream of air was bubbled through the solution for 1 hour. The reaction mixture was dried over sodium sulfate and the solvent evaporated under reduced pressure to provide the desired compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434746B2uspto-grants-2016_09