反应详情

A solution of 36.2 g of product from Example 31 in 320 ml of methyl alcohol, 125 ml ethyl alcohol, 20 ml of water and 15 g of potassium hydroxide is mechanically stirred at reflux temperature for 4 1/2 hours. The reaction is cooled and 325 ml of 1N hydrochloric acid and 200 ml of chloroform is added. The mixture is heated until homogeneous, the layers are separated and extracted with chloroform. The combined organic layers are washed with 1N hydrochloric acid, dried and concentrated in vacuo. The residue is recrystallized from chloroform/hexane to give 31 g of the product as white crystals.

1. temperatureat reflux temperature for 4 1/2 hours
2. temperatureThe reaction is cooled
3. temperatureThe mixture is heated until homogeneous, the layers
4. customare separated
5. extractionextracted with chloroform
6. washThe combined organic layers are washed with 1N hydrochloric acid
7. customdried
8. concentrationconcentrated in vacuo
9. customThe residue is recrystallized from chloroform/hexane