HRID1913427

反应详情

EQUATION

反应方程式

HRID 1913427 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

To cyano-(4-methoxy-2-nitro-phenyl)-acetic acid ethyl ester (945 mg, 3.58 mmol) was added 30 mL of a saturated solution of aqueous sodium carbonate. The mixture was stirred overnight at 55° C. After cooling to room temperature, the mixture was diluted with ethyl acetate. The organic layer was washed with saturated brine, dried over Na2SO4 and concentrated in vacuo. The crude product was purified on a Biotage (Biotage Inc.) 10 g silica column, eluting with 0-40% EtOAc in heptanes to provide 258 mg (37%) of (4-methoxy-2-nitro-phenyl)-acetonitrile.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified on a Biotage (Biotage Inc.) 10 g silica column
  6. washeluting with 0-40% EtOAc in heptanes