Reaktion #814405

ord-e12b58d967ff4497aa99e7b9739ad2ae

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool
  2. 2
    workup.ADDITIONpoured
  3. 3
    Sonstigeonto crushed ice
  4. 4
    SonstigeThe precipitate formed
  5. 5
    Filtrationis filtered off
  6. 6
    Waschenwashed with water
  7. 7
    Sonstigedried
  8. 8
    Sonstige1.06 g of white powder are thus collected
  9. 9
    SonstigeThe product is recrystallized from toluene

Vorschrift

A solution of 4.1 g (21.6 mmol) of SnCl2 in 20 ml of concentrated HCl is cooled in an ice bath. 1.32 g (5.4 mmol) of product obtained in Stage B are added gradually. The mixture is heated at 80° C. for 30 minutes. It is allowed to cool and then poured onto crushed ice. The resulting mixture is basified by addition of sodium hydroxide. The precipitate formed is filtered off, washed with water and then dried. 1.06 g of white powder are thus collected. The product is recrystallized from toluene.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05712294uspto-grants-1998_01