Реакция #501645

ord-a0ebc3a374434263b1e70ca2e35b34b5

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONwas added
  2. 2
    Температураthe mixture was heated for 24 hours at 100°-110 ° C
  3. 3
    Промывкаthe aqueous alkaline solution was washed with chloroform
  4. 4
    ФильтрацияAqueous layer was filtered
  5. 5
    ФильтрацияThe precipitate was collected by filtration
  6. 6
    Другоеrecrystalized from a mixture of dimethylformamide and ethanol affording 0.19 g of the desired compound as dark yellow crystals, m.p. 277°-282° C. (decomp.)

Методика

To a suspension of 1.13 g of 6-chloro-N-(1H-5-tetrazolyl)pyrazine-2-carboxamide in 5 ml of dimethylsulfoxide, 5.35 ml of o-toluidine was added, and the mixture was heated for 24 hours at 100°-110 ° C. Water and 10%-sodium hydroxide aqueous solution were added to the reaction mixture, and the aqueous alkaline solution was washed with chloroform. Aqueous layer was filtered and the filtrate was adjusted with 10%-hydrochloric acid to pH 3. The precipitate was collected by filtration, and recrystalized from a mixture of dimethylformamide and ethanol affording 0.19 g of the desired compound as dark yellow crystals, m.p. 277°-282° C. (decomp.).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04792547uspto-grants-1988_12