Реакция #162661

ord-b47952b60a9140c5b2852192c775aefc

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураto refluxed temperature for 2 days
  2. 2
    workup.ADDITIONwas added
  3. 3
    Другоеreaction mixture
  4. 4
    Температураwas refluxed 30 min
  5. 5
    ФильтрацияThe resulting mixture was filtered with n-butanol (100 ml)
  6. 6
    Другоеcollected solid
  7. 7
    Другоеwas dried under reduced pressure

Методика

To a stirred solution of 3-chloro-2-methylaniline (compound 26, 21.6 g, 0.15 mol) in n-butanol (200 ml) was added bis(2-chloroethyl)amine hydrochloride (compound 27, 30 g, 0.17 mol) at room temperature and allowed to refluxed temperature for 2 days. After cooled to room temperature Na2CO3 (9 g, 0.08 mol) was added and then reaction mixture was refluxed 30 min. The resulting mixture was filtered with n-butanol (100 ml) and collected solid was dried under reduced pressure to be obtained title compound (24.8 g, 81%) as a white solid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08835436B2uspto-grants-2014_09