تفاعل #466638

ord-48bb7d2fbda7478b8573f791e3da01c1

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةHeat to reflux
  2. 2
    استخلاصExtract twice with saturated aqueous solution of ammonium chloride, 5% aqueous solution of sodium bicarbonate, water, and saturated aqueous solution of sodium chloride
  3. 3
    تجفيفDry the organic layer over Na2SO4
  4. 4
    ترشيحfilter
  5. 5
    تركيزconcentrate invacuo

الإجراء التجريبي

Combine N-methyl-N-(4-(4-(1H-benzimidazole-2-carbonyl)piperidin-1-yl)-2-(3,4-dichlorophenyl)butyl)-benzamide (1.36 mmol), 2-chloroethyl ethyl ether (0.59 g, 5.44 mmol), and 1,8-diazabicyclo[5.4.0]undec-7-ene (1.66 g, 10.9 mmol) in acetonitrile (16 mL). Heat to reflux. After 18 hours, cool to ambient temperature and dilute the reaction mixture with ethyl acetate. Extract twice with saturated aqueous solution of ammonium chloride, 5% aqueous solution of sodium bicarbonate, water, and saturated aqueous solution of sodium chloride. Dry the organic layer over Na2SO4, filter, and concentrate invacuo to give the title compound.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06297259B1uspto-grants-2001_10