تفاعل #1810006

ord-4294d06dfd514258bde13d3a2d652685

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلthe methylene chloride layer is washed with water
  2. 2
    تجفيفdried over anhydrous Na2SO4
  3. 3
    أخرىEvaporation of the methylene chloride under reduced pressure
  4. 4
    أخرىaffords crude product which
  5. 5
    أخرىis purified by HPLC
  6. 6
    أخرىThe desired fractions (Rf =0.8) are evaporated
  7. 7
    أخرىto give pure free base which

الإجراء التجريبي

The title compound is prepared by adding to a stirred solution of the above sulfonyl chloride intermediate (4 g, 0.015 mol) in 50 mL of methylene chloride (2.7 g, 0.015 mol), 1-(benzyl)piperazine (2.7 g, 0.015 mol) and triethylamine (6 mL). The reactin mixture is stirred overnight and the methylene chloride layer is washed with water and dried over anhydrous Na2SO4. Evaporation of the methylene chloride under reduced pressure affords crude product which is purified by HPLC using silica gel column and ethyl acetate as the eluent. The desired fractions (Rf =0.8) are evaporated to give pure free base which is converted to the hydrochloride salt; m.p. 274°-275° C. (33% yield).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04857644uspto-grants-1989_08