Реакция #81900

Уравнение реакции

NaH

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

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

Выход 49.1%

Растворители

dimethylformamide

dimethylformamide

Условия реакции

Обработка

1. 1
   Другоеformed
2. 2
   ТемператураIt was then cooled to 50° C.
3. 3
   ТемператураThe reaction mixture was warmed
4. 4
   ТемператураUpon cooling to room temperature
5. 5
   ФильтрацияThe insoluble white product was filtered
6. 6
   Промывкаwashed with water
7. 7
   Другоеrecrystallized from ethanol

Методика

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.

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