HRID582039

反应详情

EQUATION

反应方程式

HRID 582039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a degassed r.t. solution of 2-bromo-3-(4-(methylsulfonyl)-phenyl)-2-cyclopenten-1-one (0.315 g, 1.0 mmol), Pd2 (dba)3 (0.018 g, 0.02 mmol), and AsPh3 (0.049 g, 0.16 mmol) in NMP (2.5 mL) was added a degassed NMP solution (2.5 mL) of 5-trimethylstannanyl-2-methylpyridine (~2.0 mmol). The resulting mixture was heated to 60° C. for 16 hours, then to 100° C. for a further 3.5 h. The mixture was then cooled to r.t., diluted with EtOAc, washed 2 times with 10% NH4OH and brine, dried over MgSO4, and concentrated to dryness. The residue was purified by flash chromatography (100% EtOAc/hexanes) to provide 0.070 g of the title compound as a rigid foam.

WORKUP

后处理

  1. temperatureThe mixture was then cooled to r.t.
  2. washwashed 2 times with 10% NH4OH and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated to dryness
  5. customThe residue was purified by flash chromatography (100% EtOAc/hexanes)