HRID1711972

反应详情

EQUATION

反应方程式

HRID 1711972 的结构方程式

CONDITIONS

反应条件

温度
42.5 °C

PROCEDURE

实验过程

Triethylsilane (57.2 gm) was added slowly to the reaction mixture of 5-(2-Chloro acetyl) -6-chloro oxindole (50.0 gm) and trifluoroacetic acid (175 mL) below the temperature of 45° C. The reaction was maintained at 40-45° C. for 6 hours. The reaction mass was cooled to 0° C. to -5° C. and maintained stirring for 90 minutes. The separated solid was filtered and washed with water (50 mL). Then the wet compound was further slurred in water (250 mL) for 90 minutes. The resultant solid was filtered, washed with water (50 mL) and dried at a temperature of 70-75° C. to afford 5-(2-chloroethyl) -6-chloro oxindole (43.5 gm).

WORKUP

后处理

  1. temperatureThe reaction mass was cooled to 0° C. to -5° C.
  2. temperaturemaintained
  3. filtrationThe separated solid was filtered
  4. washwashed with water (50 mL)
  5. waitThen the wet compound was further slurred in water (250 mL) for 90 minutes
  6. filtrationThe resultant solid was filtered
  7. washwashed with water (50 mL)
  8. customdried at a temperature of 70-75° C.