HRID1514411
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
4-Iodo-2-methylsulfanyl-pyrimidine (1 g, 3.97 mmol) was dissolved in dry and degassed THF (9 ml). Pd(dba)2 (114 mg, 0.20 mmol) and tri(2-furyl)phosphine (50 mg, 0.20 mmol) were added. The mixture was cooled at 0° C. and then a 0.5 M solution of 6-methyl-2-pyridylzinc bromide in THF (13 ml, 6.5 mmol) was slowly added dropwise. After stirring the mixture at room temperature for 3 hours, ethyl acetate was added and the mixture was washed with water. The organic phase was dried (Na2SO4) and evaporated. The residue was purified by flash chromatography DCM-MeOH—NH4OH (20-0.1-0.1) to give 785 mg of the title compound (90% yield).
WORKUP
后处理
- customin dry
- customdegassed THF (9 ml)
- washthe mixture was washed with water
- dry with materialThe organic phase was dried (Na2SO4)
- customevaporated
- customThe residue was purified by flash chromatography DCM-MeOH—NH4OH (20-0.1-0.1)