反応 #636130

反応方程式

hydrogen chloride

(5-bromo-2-chloropyrimidin-4-yl)-isopropylamine

3-methylsulphanylphenylamine

sodium bicarbonate

→

5-Bromo-N4-isopropyl-N2-(3-methylsulphanylphenyl)pyrimidine-2,4-diamine

溶媒

dioxane

water

acetonitrile

反応条件

後処理

1. 1
   温度After cooling
2. 2
   抽出It is extracted with ethyl acetate
3. 3
   洗浄The combined organic phases are washed with saturated sodium chloride solution
4. 4
   乾燥dried over sodium sulphate
5. 5
   その他Removal of the solvent and recrystallization of the residue from ethyl acetate/hexane 9/1
6. 6
   その他result in 0.17 g (79% of theory) of the product

実験手順

0.14 ml of a 4 molar solution of hydrogen chloride in dioxane and 0.17 ml of water are added to a solution of 0.152 g (0.61 mmol) of (5-bromo-2-chloropyrimidin-4-yl)-isopropylamine and 0.077 g (0.55 mmol) of 3-methylsulphanylphenylamine in 2 ml of acetonitrile, and the mixture is then stirred at 50° C. for 24 hours. After cooling, the mixture is added to saturated sodium bicarbonate solution. It is extracted with ethyl acetate. The combined organic phases are washed with saturated sodium chloride solution and dried over sodium sulphate. Removal of the solvent and recrystallization of the residue from ethyl acetate/hexane 9/1 result in 0.17 g (79% of theory) of the product.

出典