HRID12615

反应详情

EQUATION

反应方程式

HRID 12615 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To methanol (10 mL), thionyl chloride (0.76 mL) was added dropwise at −15 to −10° C., followed by stirring for 30 minutes. To the mixture, (4-bromo-1H-indol-3-yl)acetic acid (Chemical and Pharmaceutical Bulletin, 33(9), 3696-3708 (1985), 1.32 g) was added, followed by stifling at room temperature for 2 hours. To the reaction mixture, an aqueous saturated sodium hydrogen carbonate solution was added, followed by extraction with ethyl acetate. The organic layer was washed in turn with water and saturated saline, dried and then concentrated. The residue was washed with diisopropyl ether/n-hexane (1:2) to obtain the titled compound having the following physical properties (1.26 g).

WORKUP

后处理

  1. waitby stifling at room temperature for 2 hours
  2. extractionfollowed by extraction with ethyl acetate
  3. washThe organic layer was washed in turn with water and saturated saline
  4. customdried
  5. concentrationconcentrated
  6. washThe residue was washed with diisopropyl ether/n-hexane (1:2)