HRID1095908
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
- 100 °C
PROCEDURE
实验过程
Triethyl amine (0.02 ml), 4-vinylbenzoic acid (CAS Reg. No. 1075-49-6, 19 mg), tri-o-tolylphosphine (2 mg) and palladium acetate (1 mg) were added to a solution of 3-(4-bromo-2-chloro-phenyl)-1,1,1-trifluoro-2-(2-methyl-pyridin-4-yl)-butan-2-ol (Example 60 step 1, 41 mg) in DMF (1 ml). The mixture was stirred at 100° C. for 3 h. Water was added and extracted with EtOAc. The combined organic layers were dried over Na2SO4 and then concentrated to an oil. The residue was purified by flash chromatography (SiO2, 0->100% EtOAc/heptane) to give the title compound (28 mg) as an orange oil. MS (m/e)=476.1 [M+H+].
WORKUP
后处理
- extractionextracted with EtOAc
- dry with materialThe combined organic layers were dried over Na2SO4
- concentrationconcentrated to an oil
- customThe residue was purified by flash chromatography (SiO2, 0->100% EtOAc/heptane)