تفاعل #3260

معادلة التفاعل

NaH

2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7-ol

methyl iodide

→

2-amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3-d]pyrimidin-7(8H)-one

المردود 49.1%

المذيبات

dimethylformamide

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   أخرىformed
2. 2
   درجة الحرارةIt was then cooled to 50° C.
3. 3
   درجة الحرارةThe reaction mixture was warmed
4. 4
   درجة الحرارةUpon cooling to room temperature
5. 5
   ترشيحThe insoluble white product was filtered
6. 6
   غسيلwashed with water
7. 7
   أخرىrecrystallized from ethanol

الإجراء التجريبي

To a mixture of 2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7-ol (3.7 g) from Example 11 in dimethylformamide was added NaH (50% suspension in mineral oil, 0.64 g). The resulting slurry was heated at 65° C. for 0.5 hour until a solution formed. It was then cooled to 50° C. and a solution of methyl iodide (2.0 g) in dimethylformamide (10 mL) was added dropwise to the reaction. The reaction mixture was warmed and kept between 60° C.-80° C. for 3 hours. Upon cooling to room temperature, the reaction mixture was poured into ice water. The insoluble white product was filtered, washed with water, and recrystallized from ethanol using charcoal to give 1.9 g of 2-amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3-d]pyrimidin-7(8H)-one; mp 235°-237° C.

المصدر