Reaktion #2028887

ord-9b9dc4fd40474022806e97056924a4ff

Reaktionsgleichung

Cl
hydrochloric acid
CCOC=O
Ethyl formate
CC(=O)c1ccc(Cl)cc1
4′-chloroacetophenone
C[O-].[Na+]
Sodium methoxide
O=CCC(=O)c1ccc(Cl)cc1
yellow oil
Ausbeute 100.2%
O=CCC(=O)c1ccc(Cl)cc1
3-[4-(chloro)phenyl]-propane-1,3-dione
Ausbeute 100.2%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe phases were separated
  2. 2
    Waschenthe ethereal solution washed with brine
  3. 3
    Trocknendried over magnesium sulfate
  4. 4
    Filtrationfiltered
  5. 5
    Einengenconcentrated in vacuo

Vorschrift

Ethyl formate (8.15 g, 0.11 mol) and 4′-chloroacetophenone (15.4 g, 0.1 mol) were stirred in ether (150 mL) at room temperature. Sodium methoxide (25%) (23.77 g, 0.11 mol) was added dropwise. The mixture was stirred at room temperature for 16 hours and was then treated with 150 mL of 1N hydrochloric acid. The phases were separated and the ethereal solution washed with brine, dried over magnesium sulfate, filtered and concentrated in vacuo to afford 18.3 g of a yellow oil. The resulting crude mixture was used directly in the next step without purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: USRE044048E1uspto-grants-2013_03