HRID2242222

反应详情

EQUATION

反应方程式

HRID 2242222 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-chloro-5-[5-(4-isobutylphenyl)-1,2,4-oxadiazol-3-yl]pyridine (5.0 g, 16.0 mmol), zinc cyamide (1.13 g, 9.58 mmol), tetrakis(triphenylphosphine) palladium (0) (0.74 g, 0.64 mmol) and DMF (16 mL) was stirred at 80° C. for 24 hours. The reaction mixture was cooled to room temperature, quenched with H2O (10 mL), and extracted with EtOAc (3×100 mL). The combined organic extracts were washed with H2O (2×100 mL) and brine (2×100 mL), dried (MgSO4), filtered and concentrated in vacuo. Purification by flash chromatography (silica, 2:8 EtOAc:hexanes) provided the title compound (2.87 g, 59% yield) as a solid.

WORKUP

后处理

  1. customquenched with H2O (10 mL)
  2. extractionextracted with EtOAc (3×100 mL)
  3. washThe combined organic extracts were washed with H2O (2×100 mL) and brine (2×100 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customPurification by flash chromatography (silica, 2:8 EtOAc:hexanes)