Reaktion #355441

ord-457f7c366ff64050bad93c547817cb8f

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONA mixture of 40 g
  2. 2
    Temperaturat reflux
  3. 3
    EinengenThe reaction was concentrated to dryness in vacuo
  4. 4
    SonstigeThe product was recrystallized from 800 ml
  5. 5
    Sonstigeof MeOH, to give 28 m
  6. 6
    Sonstige258°-293°C
  7. 7
    SonstigeA second recrystallization from 1000 ml
  8. 8
    Sonstigeof MeOH gave m.p. 257°-260°C.

Vorschrift

A mixture of 40 g. (0.184 m.) of the compound of Example I, C., 282 g. (0.184 m.) of 2,5-dimethoxyaniline and 500 ml. of ethanol was heated at reflux with stirring overnight. The reaction was concentrated to dryness in vacuo. The product was recrystallized from 800 ml. of MeOH, to give 28 m.p. 258°-293°C. A second recrystallization from 1000 ml. of MeOH gave m.p. 257°-260°C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US03947434uspto-grants-1976_03