HRID659100

反应详情

EQUATION

反应方程式

HRID 659100 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

2-Bromo-6-phenyl-pyridine (13) (100 mg, 0.43 mmol), K2CO3 (117 mg, 0.85 mmol) in acetone (2 mL) was added 3-bromothiophenol and the reaction mixture was heated in a CEM Discover microwave for 1×30 minutes at 90° C., then 4×2 hours at 130° C., followed by 1×8 hours at 130° C. The crude product was partially purified by column chromatography eluting with 10% EtOAc in heptane to give the title compound. Yield: 100 mg, 68%; LC-MS tr 1.97 min; HPLC Purity: 55%; MS (ES+) m/z 342, 344 (M+H)

WORKUP

后处理

  1. custom4×2 hours
  2. customat 130° C.
  3. customfollowed by 1×8 hours at 130° C
  4. customThe crude product was partially purified by column chromatography
  5. washeluting with 10% EtOAc in heptane