Reaktion #51667

ord-ffe6f370f9a649a1b163cc5fc18bcff1

Reaktionsbedingungen

Temperatur
120°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated in an oil bath
  2. 2
    workup.STIRRINGThe homogeneous solution was stirred at this temperature for 90 minutes
  3. 3
    Temperaturto cool to room temperature
  4. 4
    SonstigeThe flask was immersed in an ice bath
  5. 5
    workup.ADDITIONthe suspension of the product
  6. 6
    workup.STIRRINGwas stirred at this temperature until all was crystalline
  7. 7
    FiltrationFiltration
  8. 8
    Waschenwashing well with water
  9. 9
    Sonstigethorough drying

Vorschrift

The crystalline N-(2-Chloro-6-methanesulfonylmethyl-phenyl)-2,2,2-trifluoro-acetamide of Step 3 was taken up into 200 ml of 2N solution of sodium hydroxide and stirred and heated in an oil bath heated to 120° C. The homogeneous solution was stirred at this temperature for 90 minutes and slowly allowed to cool to room temperature. The flask was immersed in an ice bath and the suspension of the product was stirred at this temperature until all was crystalline. Filtration, washing well with water and thorough drying afforded 13.96 g of pure crystalline 2-chloro-6-methanesulfonylmethyl-phenylamine (90%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06852726B2uspto-grants-2005_02