HRID2295908

反应详情

EQUATION

反应方程式

HRID 2295908 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 200 ml. of butanol was added 40.3 g. of potassium hydroxide containing about 14% of water, and the mixture was stirred at ambient temperature to obtain a gelatinous mixture. To it was added 20 g. of 1,1,1-trichloro-2-(3-trifluoromethylphenyl)ethane, over about 5 minutes. The mixture was then heated to reflux and stirred at that temperature for 5 hours. It was then cooled and worked up as described in Example 1 above. The major product was distilled at 89°-97° under 0.5-0.7 torr to obtain 12.8 g. of the desired product. It was analyzed by vapor phase chromatography, using a 180-cm. column packed with Chrom G silica gel coated with 1.5% of OV-17 and 1.95% of OV-210, and found to be 94.0% pure.

WORKUP

后处理

  1. customto obtain a gelatinous mixture
  2. additionTo it was added 20 g
  3. temperatureThe mixture was then heated
  4. temperatureto reflux
  5. temperatureIt was then cooled
  6. distillationThe major product was distilled at 89°-97° under 0.5-0.7 torr
  7. customto obtain 12.8 g