Reacción #524332

ord-e3f389eca53b4245b0739a11d99ecfad

Ecuación de reacción

NS(=O)(=O)c1cc(C(=O)O)c(Cl)cc1F
6-chloro-4-fluoro-3-sulfamoylbenzoic acid
CCCCN1CCNCC1
N-butylpiperazine
CCCCN1CCN(c2cc(Cl)c(C(=O)O)cc2S(N)(=O)=O)CC1
4-(4-n-butylpiperazine-1-yl)-6-chloro-3-sulfamoylbenzoic acid

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otroa small amount of amorphous precipitate formed
  2. 2
    Otrowas separated
  3. 3
    Filtraciónthe crystalline precipitate was suction-filtered
  4. 4
    Otrowas recrystallized from a mixture of ethanol and water

Procedimiento

126 Grams of 6-chloro-4-fluoro-3-sulfamoylbenzoic acid (0.5 mole) were stirred with 0.2 l of N-butylpiperazine for 2 hours at 110° C. Subsequently the reaction solution was poured into 2 l of water, a small amount of amorphous precipitate formed was separated, and the filtrate was adjusted to a pH of 7.5 with 2N HCl. After having stood overnight at room temperature, the crystalline precipitate was suction-filtered and was recrystallized from a mixture of ethanol and water.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04029787uspto-grants-1977_06