반응 #81900

반응 방정식

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

수율 49.1%

용매

dimethylformamide

dimethylformamide

반응 조건

후처리

1. 1
   기타formed
2. 2
   온도It was then cooled to 50° C.
3. 3
   온도The reaction mixture was warmed
4. 4
   온도Upon cooling to room temperature
5. 5
   여과The insoluble white product was filtered
6. 6
   세척washed with water
7. 7
   기타recrystallized from ethanol

실험 절차

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.

출처