HRID863299

反应详情

EQUATION

反应方程式

HRID 863299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 3.15 g of ethyl indole-3-carboxylate, 4.36 g of di-tert-butylcarbonate and 0.02 g of 4-DMAP in 30 ml of acetonitrile is stirred at room temperature for 15 min. The reaction mixture is then diluted with 200 ml of ethyl acetate. The organic phase is washed with dilute hydrochloric acid, water and saturated sodium chloride solution in succession, dried over sodium sulfate and concentrated. Purification by means of FC over 80 g of silica gel with a 15:1 mixture of hexane and ethyl acetate as the mobile phase gives 5.1 g of the title compound: Rf (G)=0.41.

WORKUP

后处理

  1. washThe organic phase is washed with dilute hydrochloric acid, water and saturated sodium chloride solution in succession
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated
  4. customPurification by means of FC over 80 g of silica gel
  5. additionwith a 15:1 mixture of hexane and ethyl acetate as the mobile phase