Reacción #5887

ord-a9b6c5936caf4afa829011ebb019f26e

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    FiltraciónAfter filtering off the solid
  2. 2
    Otrothe solution is evaporated
  3. 3
    Otroto get a yellow solid which
  4. 4
    OtroThe solid separated
  5. 5
    Extracciónis extracted with hexane
  6. 6
    Filtraciónfiltered through 150 g of neutral alumina

Procedimiento

To a stirred mixture of 75 g of 6-Amino-2-tert-butyl-5-(4-methylpiperazin-1-yl)benzothiazole and 29 g of sodium bicarbonate in 1100 ml of chloroform at 0° is added 41 g of thiophosgene and the mixture stirred at 10° for 4 hours. After filtering off the solid, the solution is evaporated to get a yellow solid which is dissolved in water and the pH of the solution is brought to 7 by the addition of dilute sodium hydroxide. The solid separated is extracted with hexane and filtered through 150 g of neutral alumina to give 2-tert-butyl-6-isothiocyanato-5-(4-methyl-piperazin-1-yl)benzothiazole, melting at 124°-126°.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05246927uspto-grants-1993_09