反应详情

A mixture of 25 g of product from Example 109, 11.54 g of potassium hydroxide, 30 ml of water and 500 ml ethyl alcohol is heated at reflux temperature for 24 hours. The reaction mixture is cooled and maintained at room temperature for 48 hours. The mixture is acidified to pH 2 with concentrated hydrochloric acid, concentrated in vacuo, diluted with water and extracted with chloroform. The combined chloroform extracts are washed with saturated sodium chloride, dried and concentrated in vacuo to give 22.58 g of the desired product as colorless crystals.

1. temperatureis heated
2. temperatureat reflux temperature for 24 hours
3. temperatureThe reaction mixture is cooled
4. concentrationconcentrated in vacuo
5. additiondiluted with water
6. extractionextracted with chloroform
7. washThe combined chloroform extracts are washed with saturated sodium chloride
8. customdried
9. concentrationconcentrated in vacuo