反応 #3260

反応方程式

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

収率 49.1%

溶媒

dimethylformamide

dimethylformamide

反応条件

後処理

1. 1
   その他formed
2. 2
   温度It was then cooled to 50° C.
3. 3
   温度The reaction mixture was warmed
4. 4
   温度Upon cooling to room temperature
5. 5
   ろ過The insoluble white product was filtered
6. 6
   洗浄washed with water
7. 7
   その他recrystallized from ethanol

実験手順

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.

出典