HRID502106

反应详情

EQUATION

反应方程式

HRID 502106 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 6-methoxy-1H-indole-3-carbonitrile (9.9 g, 57.6 mmol) in DMF (150 mL) is added NaH (60% dispersion in mineral oil, 3.45 g, 86.3 mmol). The reaction mixture is stirred for 15 min and then ethyl iodide (5.53 mL, 69.1 mmol) is added and the mixture is stirred at room temperature overnight. The reaction mixture is then diluted with H2O and extracted with EtOAc (2×). The organic phases are washed with H2O (3×) and saturated NaCl and then dried and concentrated to a semi-solid. The crude product is purified via column chromatography on silica gel (200 g) using CH2Cl2/hexanes (50-100%) as eluent to yield 6-methoxy-1-ethyl-1H-indole-3-carbonitrile as a tan solid.

WORKUP

后处理

  1. stirringthe mixture is stirred at room temperature overnight
  2. extractionextracted with EtOAc (2×)
  3. washThe organic phases are washed with H2O (3×) and saturated NaCl
  4. customdried
  5. concentrationconcentrated to a semi-solid
  6. customThe crude product is purified via column chromatography on silica gel (200 g)