HRID631879

反应详情

EQUATION

反应方程式

HRID 631879 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperatureThe mixture was cooled
  2. custompartitioned between water and DCM
  3. customThe organic solution was separated
  4. dry with materialdried with magnesium sulfate
  5. filtrationfiltered
  6. customthe solvent was removed under vacuum
  7. customThe residue was purified by flash chromatography on silica
  8. washeluting with a mixture of ethyl acetate and cyclohexane
  9. additionThe fractions containing the desired product
  10. customevaporated