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
2-Bromo-6-nitrobenzonitrile (0.56 g), cyclopropyl boronic acid (0.63 g), palladium (II) acetate (0.055 g), tricyclohexylphosphine (0.135 g) and potassium phosphate tribasic (2.36 g) were dissolved in a mixture of toluene (15 mL) and water (3 mL). The mixture was heated at 100° C. under nitrogen for 18 hours. The mixture was cooled and then partitioned between water and DCM. The organic solution was separated, dried with magnesium sulfate, filtered and the solvent was removed under vacuum. The residue was purified by flash chromatography on silica, eluting with a mixture of ethyl acetate and cyclohexane. The fractions containing the desired product were combined and evaporated to give the title compound as a light yellow solid (0.51 g).
WORKUP
后处理
- temperatureThe mixture was cooled
- custompartitioned between water and DCM
- customThe organic solution was separated
- dry with materialdried with magnesium sulfate
- filtrationfiltered
- customthe solvent was removed under vacuum
- customThe residue was purified by flash chromatography on silica
- washeluting with a mixture of ethyl acetate and cyclohexane
- additionThe fractions containing the desired product
- customevaporated