Reaktion #992015

ord-178e81cbbb4f43ab9b2dfbb3251c0399

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA small amount of solid precipitate was removed by filtration
  2. 2
    workup.ADDITIONportion of N-chlorosuccinimide was added to the filtrate
  3. 3
    workup.ADDITIONportion of N-chlorosuccinimide was then added to the reaction mixture
  4. 4
    workup.STIRRINGstirring
  5. 5
    workup.WAITwas continued for twelve hours
  6. 6
    SonstigeThe white precipitate which had formed
  7. 7
    Filtrationwas collected by filtration and air
  8. 8
    Sonstigedried
  9. 9
    Sonstigeto give 640 mg

Vorschrift

A solution of 1.0 g of 1-(thiazin-2-yl)-2-amino-6-(α-methylenebenzyl)benzimidazole in 50 ml. of tetrahydrofuran containing 500 mg. of N-chlorosuccinimide stood at room temperature for twelve hours. A small amount of solid precipitate was removed by filtration. An additional 500 mg. portion of N-chlorosuccinimide was added to the filtrate and the solution was stirred for six hours at room temperature. Another 500 mg. portion of N-chlorosuccinimide was then added to the reaction mixture and stirring was continued for twelve hours. The white precipitate which had formed was collected by filtration and air dried to give 640 mg. (57%) of 1-(thiazin-2-yl)-2-amino-6-(α-dichloromethylenebenzyl)benzimidazole hydrochloride. M.P. 214°-217° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04420479uspto-grants-1983_12