Reaktion #40770

ord-d84e1cfa1e914306a388d7fad0ad38b1

Lösungsmittel

Reaktionsbedingungen

Temperatur
40°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture was refluxed for 5 h
  2. 2
    Temperaturwas cooled further to 20° C
  3. 3
    FiltrationThe precipitate was filtered
  4. 4
    Waschenwashed with acetone and PA, and air
  5. 5
    Sonstigedried

Vorschrift

To EtOH (80 mL), p-chloroacetophenone (77.3 g, 0.50 mol), dimethylamine hydrochloride (52.7 g, 0.65 mol), paraformaldehyde (19.8 g, 0.66 mol) and concentrated aqueous HCl (1 mL) were added and the mixture was refluxed for 5 h. The mixture was cooled to 40° C., acetone (400 mL) was added, and under stirring the mixture was cooled further to 20° C. The precipitate was filtered, washed with acetone and PA, and air dried to obtain 69.5 g of product which was used without further purification in the subsequent step.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07728018B2uspto-grants-2010_06