تفاعل #3282
ord-a8f31c3f69e44f889459e4fbf80bb158
معادلة التفاعل
المتفاعلات
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
110°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةwas heated
- 2درجة الحرارةAfter 20 hours reflux
- 3أخرىthe excess amine and dimethylformamide were evaporated
- 4أخرىthe residue was triturated with water
- 5ترشيحfiltered
- 6غسيلwashed with water
- 7أخرىdried
- 8أخرىRecrystallization from ethyl acetate/petroleum ether
- 9أخرىgave pure product
الإجراء التجريبي
A mixture of 0.177 g (0.50 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 37, 10 mL of n-butylamine and 1.0 mL of dimethylformamide was heated with stirring to reflux (110° C. oil bath). After 1 hour, solution was complete. After 20 hours reflux, the excess amine and dimethylformamide were evaporated, and the residue was triturated with water, filtered, washed with water, and dried; wt 0.180 g. Recrystallization from ethyl acetate/petroleum ether gave pure product; wt 0.116 g; mp 184°-186° C.