تفاعل #318297

ord-a1a9c68ba756471fa71dd3bf7f89da53

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    أخرىReaction
  3. 3
    أخرىseparated
  4. 4
    درجة الحرارةwhilst heating
  5. 5
    درجة الحرارةThe mixture was cooled
  6. 6
    ترشيحthe crystals were collected by filtration
  7. 7
    أخرىrecrystallized from acetone

الإجراء التجريبي

3.6 g of 4-{2-[4-(2-ethoxyethyl)-2-methylphenoxy]ethylamino}thieno[2,3-d]pyrimidine were dissolved in 30 ml of acetone, and 0.9 g of anhydrous oxalic acid dissolved in 30 ml of acetone was added thereto. Reaction occurred at once, and crystals separated. The mixture was stirred for a further 30 minutes whilst heating. The mixture was cooled, and the crystals were collected by filtration and recrystallized from acetone to give 3.9 g of the title compound as colorless columnar crystals melting at 151°-152° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04845097uspto-grants-1989_07