Reaktion #739952

ord-4e06245e642845d484cf9dc172ee93e1

Lösungsmittel

Reaktionsbedingungen

Temperatur
85°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigefitted with an agitator
  2. 2
    Sonstigeto reach 40° C
  3. 3
    Temperaturcooled
  4. 4
    FiltrationThe precipitate which forms is filtered
  5. 5
    Waschenwashed with water
  6. 6
    Sonstigedried in an oven at 50° C.

Vorschrift

260 g of 2-methoxy-4-amino-5-methyl-thio-benzoic acid and 520 ml of acetic acid are placed in a 2 liter flask fitted with an agitator, a thermometer, a condenser and a dropping funnel. 123 ml of acetic anhydride (density 1.082) is poured in slowly. The temperature rises to reach 40° C. The reaction mixture is heated for 1 hour 30 at 85° C., cooled and poured over 1,000 g of ice and 1,000 ml of water. The precipitate which forms is filtered, washed with water and dried in an oven at 50° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04673686uspto-grants-1987_06