HRID7700

反应详情

EQUATION

反应方程式

HRID 7700 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

To a stirred solution of 4-bromo-2-fluoro benzyl bromide (1.5 g, 5.6 mmol) in DMF (50 mL) was added sodium cyanide (0.8 g, 16.8 mmol). The reulting reaction mixture was stirred at 90° C. for 1 h, cooled to rt, quenched with brine (50 mL) and extracted with EtOAc (3×100 mL). The organic layers were combined, washed with brine (50 mL), dried (MgSO4) and concentrated in vacuo. The residue was purified by flash column (silica gel, hexanes:EtOAc 5:1) to afford 4-bromo-2-fluoro benzyl cyanide as yellow solid. MS (ESI) 307 (M+H)+.

WORKUP

后处理

  1. customThe reulting reaction mixture
  2. temperaturecooled to rt
  3. customquenched with brine (50 mL)
  4. extractionextracted with EtOAc (3×100 mL)
  5. washwashed with brine (50 mL)
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by flash column (silica gel, hexanes:EtOAc 5:1)