Reacción #93400

ord-aa7ce148d31c4b488ae35901f579ecc8

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.WAITAfter a further hour at 50°
  2. 2
    Filtraciónthe precipitated product is filtered off
  3. 3
    workup.DISSOLUTIONdissolved in dilute sodium hydroxide solution
  4. 4
    FiltraciónThe solution is filtered
  5. 5
    FiltraciónThe precipitate is filtered off
  6. 6
    Otrodried at 60° in vacuo

Procedimiento

16.8 g of finely powdered 2-mercaptobenzothiazole are suspended in 40 ml of 70% sulfuric acid, and 10.2 g of powdered maleic anhydride are added at 48°-51° in the course of 1 hour, with stirring. After a further hour at 50°, the reaction mixture is cooled to room temperature and is diluted by dropwise addition of 250 ml of water at 25°-35°. After 1 hour, the precipitated product is filtered off and dissolved in dilute sodium hydroxide solution. The solution is filtered and the filtrate is acidified with hydrochloric acid. The precipitate is filtered off and dried at 60° in vacuo. 24.7 g (87% of theory) of benzothiazol-2-ylthiosuccinic acid of melting point 175°-176°, with decomposition, are thus obtained.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04612378uspto-grants-1986_09