HRID2194882

反应详情

EQUATION

反应方程式

HRID 2194882 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

KCN (1.1 eq.) was added to a stirred solution of (2′-chloro-3-methylbiphenyl-4-yl)methyl methanesulfonate (1 eq.) from step 2 in DMF (0.13M). The suspension was stirred 12 h. at 80° C. The final mixture was cooled down to room temperature, poured in water and extracted with Et2O. The organic extract was washed with water (2×), brine, dried over MgSO4, filtered and concentrated. The residue was purified by column chromatography on silica gel (Combi-Flash by ISCO), eluting with Hex/EtOAc (0 to 50% in 30 min) to afforded the desired compound as a beige solid.

WORKUP

后处理

  1. extractionextracted with Et2O
  2. extractionThe organic extract
  3. washwas washed with water (2×), brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified by column chromatography on silica gel (Combi-Flash by ISCO)
  8. washeluting with Hex/EtOAc (0 to 50% in 30 min)