تفاعل #2091
ord-2b41b35df72e44c4adc18e6e041d2837
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةheated at 120° C. for a further 6 hours
- 2درجة الحرارةThe reaction mixture was cooled
- 3ترشيحThe solid was filtered off with suction
- 4غسيلwashed with water
- 5ترشيحThe crystallizate was filtered
- 6غسيلwashed with ethanol
- 7أخرىdried 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.