Reaktion #1946546

ord-158dae43966a4dd5b0fc23a9a3e6ced4

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAITfor an additional 6 hours at room temperature
  2. 2
    workup.ADDITIONThe reaction mixture is then poured into 800 g
  3. 3
    SonstigeThe solid product precipitates from solution
  4. 4
    Filtrationis collected by filtration
  5. 5
    Sonstigeair dried at room temperature
  6. 6
    Sonstigeto afford A-4-MASA in quantitative yield

Vorschrift

A few drops of concentrated sulfuric acid is added to a stirring solution of 35.0 g of 4-methacrylamidosalicylic acid (prepared according to Example 1) in 350 mL of acetic anhydride at 0° C. The solution is stirred for 60 minutes at 0° C. and then for an additional 6 hours at room temperature. The reaction mixture is then poured into 800 g of cold deionized water. The solid product precipitates from solution, and is collected by filtration. The product is then air dried at room temperature to afford A-4-MASA in quantitative yield.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06527959B1uspto-grants-2003_03