تفاعل #357015

ord-08fe5b294aa04e7e99b34cf0879f4d24

المذيبات

ظروف التفاعل

درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe reaction mixture was cooled down to room temperature
  2. 2
    ترشيحthe precipitated solid was collected by filtration
  3. 3
    غسيلwashed with water and methanol
  4. 4
    أخرىBy recrystallizing the resulting solid from a THF-methanol mixed solvent

الإجراء التجريبي

A 15 ml THF-methanol (1:1) solution of 750 mg of ethyl 1-(4-{[5-(aminocarbonyl)-4-(benzylamino)pyrimidin-2-yl]amino}phenyl)piperidine-4-carboxylate was mixed with 1 M sodium hydroxide aqueous solution, followed by stirring under heating at 60° C. for 1 hour. The reaction mixture was cooled down to room temperature and mixed with 1 M sodium hydroxide aqueous solution, and the precipitated solid was collected by filtration and washed with water and methanol. By recrystallizing the resulting solid from a THF-methanol mixed solvent, 361 mg of 1-(4-{[5-(aminocarbonyl)-4-(benzylamino)pyrimidin-2-yl]amino}phenyl)piperidine-4-carboxylic acid was obtained as a colorless solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07449456B2uspto-grants-2008_11