Реакция #44164

ord-464650e679c244c79fcc98e28eb181ec

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.STIRRINGThe mixture was stirred for 90 minutes
  2. 2
    Другоеpurified by ion exchange chromatography [SCX-2; MeOH-(1M NH3/MeOH): (100:0)→(0:100)]
  3. 3
    КонцентрированиеThe basic washings were concentrated in vacuo
  4. 4
    Другоеpurified by column chromatography [SiO2; cyclohexane-EtOAc-MeOH: (1:1:0)→(0:10:1)]

Методика

To a stirred solution of 1-(3-{2-[4-(2-methyl-5-quinolinyl)-1-piperazinyl]ethyl}phenyl)-2-imidazolidinone (Example 85, 50 mg) in DMF (1 mL) was added sodium hydride (60%, 10 mg). The mixture was stirred for 15 minutes, then iodoethane (11 L) was added. The mixture was stirred for 90 minutes then diluted with methanol (5 mL) and purified by ion exchange chromatography [SCX-2; MeOH-(1M NH3/MeOH): (100:0)→(0:100)]. The basic washings were concentrated in vacuo and purified by column chromatography [SiO2; cyclohexane-EtOAc-MeOH: (1:1:0)→(0:10:1)] and converted to the hydrochloride salt according to the description given in the general procedure (D6) to give the title compound (49 mg).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07732600B2uspto-grants-2010_06