반응 #636130

반응 방정식

hydrogen chloride

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

3-methylsulphanylphenylamine

sodium bicarbonate

→

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

용매

dioxane

water

acetonitrile

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   추출It is extracted with ethyl acetate
3. 3
   세척The combined organic phases are washed with saturated sodium chloride solution
4. 4
   건조dried over sodium sulphate
5. 5
   기타Removal of the solvent and recrystallization of the residue from ethyl acetate/hexane 9/1
6. 6
   기타result in 0.17 g (79% of theory) of the product

실험 절차

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.

출처