反应详情

In 10 ml of tetrahydrofuran was suspended 1.3 g of zinc (powder), to which dibromoethane (2 drops) was added. The mixture was heated under reflux for 5 minutes, to which trimethylsilane chloride was added. The mixture was further heated under reflux for 5 minutes, to which a solution of 2.4 g of 2-chloro-5-methyl-6-fluorobenzyl bromide dissolved in 20 ml of tetrahydrofuran was slowly added with heating under reflux, followed by stirring for 20 minutes. (The solution thus obtained is referred to as solution 0). In 10 ml of tetrahydrofuran were suspended 1.5 g of 4,6-dichloropyrimidine and 0.1 g of dichlorobistriphenylphosphine palladium, to which the above solution L was added, followed by heating under reflux for 3 hours and further stirring at room temperature for 12 hours. The reaction mixture was then poured into water and extracted three times with ethyl acetate. The organic layers were combined, washed with water, dried over anhydrous magnesium sulfate, and then concentrated. The residue was subjected to silica gel column chromatography to give 0.53 g of 4-chloro-6-(2-chloro-5-methyl-6-fluorobenzyl)pyrimidine.

1. temperatureThe mixture was heated
2. additionwas added
3. temperatureThe mixture was further heated
4. additionwas slowly added
5. temperaturewith heating
6. temperatureunder reflux
7. custom(The solution thus obtained
8. temperatureby heating
9. temperatureunder reflux for 3 hours
10. stirringfurther stirring at room temperature for 12 hours
11. extractionextracted three times with ethyl acetate
12. washwashed with water
13. dry with materialdried over anhydrous magnesium sulfate
14. concentrationconcentrated