HRID440333

反应详情

EQUATION

反应方程式

HRID 440333 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Bromothiazole (1.2 mmol, 0.11 mL) and phenylboric acid (1.2 mmol, 0.146 g) were added to a solution of potassium carbonate (2M, 1.2 mL) and ethanol (0.6 mL) in deoxygenated toluene (12 mL). The resulting mixture was degassed for 30 minutes, then tetrakistriphenylphosphine palladium (0.036 mmol, 0.042 g) was added and the solution heated at reflux for 48 hours. The solids were removed by filtration and the solution extracted with toluene (5x), dried (MgSO4), filtered and concentrated. The residue was subjected to flash chromatography (hexane followed with 5% ethyl acetate/hexane and then 10% ethyl acetate/hexane) to afford 0.13 g (69%) of 2-phenylthiazole.

WORKUP

后处理

  1. customThe resulting mixture was degassed for 30 minutes
  2. temperaturethe solution heated
  3. temperatureat reflux for 48 hours
  4. customThe solids were removed by filtration
  5. extractionthe solution extracted with toluene (5x)
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated