تفاعل #2091

ord-2b41b35df72e44c4adc18e6e041d2837

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةheated at 120° C. for a further 6 hours
  2. 2
    درجة الحرارةThe reaction mixture was cooled
  3. 3
    ترشيحThe solid was filtered off with suction
  4. 4
    غسيلwashed with water
  5. 5
    ترشيحThe crystallizate was filtered
  6. 6
    غسيلwashed with ethanol
  7. 7
    أخرىdried under reduced pressure

الإجراء التجريبي

16.8 g (0.7 mol) of sodium hydride were introduced in portions with stirring into a suspension of 99.6 g (0.6 mol) of 3-methylxanthine in 1.5 l of dimethylformamide. After evolution of hydrogen had ended, the mixture was heated to 100° C., treated dropwise with 76 g (0.6 mol) of benzyl chloride and heated at 120° C. for a further 6 hours. The reaction mixture was cooled and cautiously poured into 3 l of water. The solid was filtered off with suction and washed with water, the filter residue was taken up in ethanol and the solution was stirred at room temperature for one hour. The crystallizate was filtered, washed with ethanol and dried under reduced pressure.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05728686uspto-grants-1998_03