HRID1250031

反应详情

EQUATION

反应方程式

HRID 1250031 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(4-flourophenyl)-3-acetoxy-5-chloroindole (100.0 g, 0.33 mol) was dissolved in 1000 mL EtOH. During the next hour sodium borohydride pellets (18.7 g, 1.5 eq.) were added batchwise at reflux. The reaction mixture was stirred over night at reflux and cooled to room temperature. Concentrated HCl (appr. 50 mL until pH 1) was added and the reaction mixture was stirred at room temperature for 1 hour. 200 mL demineralized water was added, and the resulting suspension was filtrated. The filter cake was washed with further 50 mL water and 10 mL EtOH. The product was dried over night in vacuum at 50° C.

WORKUP

后处理

  1. temperatureat reflux
  2. temperatureat reflux
  3. stirringthe reaction mixture was stirred at room temperature for 1 hour
  4. additionwas added
  5. filtrationthe resulting suspension was filtrated
  6. washThe filter cake was washed with further 50 mL water and 10 mL EtOH
  7. customThe product was dried over night in vacuum at 50° C.