反应详情

温度

97.5 °C

4 g of 4-[1-(2-ethoxy-ethyl)-1H-indol-3-yl]-piperidine-1-carboxylic acid ethyl ester and 3.81 g of potassium hydroxide 85% were added to 14 g of 2-propanol and the mixture was heated at 95-100° C. for 16 hours. The solvent was distilled off and water was added. The mixture was extracted with toluene and the organic layer was separated, washed with water and concentrated. The residue was disolved in a mixture of 10 mL of ethyl alcohol 96% and 6 mL of 2-propanol and 1.4 g of fumaric acid were added. The mixture was refluxed for 30 minutes. After cooling at 0-5° C. for 30 minutes the formed solid was isolated by suction filtration. 4.05 g of a white solid were recovered as a salt of the product with fumaric acid.

1. distillationThe solvent was distilled off
2. additionwater was added
3. extractionThe mixture was extracted with toluene
4. customthe organic layer was separated
5. washwashed with water
6. concentrationconcentrated
7. additionThe residue was disolved in a mixture of 10 mL of ethyl alcohol 96% and 6 mL of 2-propanol and 1.4 g of fumaric acid
8. additionwere added
9. temperatureThe mixture was refluxed for 30 minutes
10. temperatureAfter cooling at 0-5° C. for 30 minutes the formed solid
11. customwas isolated by suction filtration
12. custom4.05 g of a white solid were recovered as a salt of the product with fumaric acid