反应详情

温度

60 °C

Place 100 g of 4-phenylpiperidine-4-carboxylic acid and p-toluenesulphonic acid in 800 ml of dioxane, add 150 ml of water and 109.7 g of K2CO3. Heat to 60° C. then add, drop by drop, 60.7 g of (Boc)20 in 100 ml of dioxane. Leave for 4 hours with stirring at 60° C. then heat under reflux for 1 hour. Evaporate to dryness, take up the solid formed in water, acidify to a pH of 3 by the addition of 2 N HCl, then add ether. Filter the crystals formed, wash them in water then in ether. Evaporate the etherified filtrate to dryness, take up the residue in ether and filter the crystals formed and add to those already obtained in order to dry them. 71 g of the desired compound are obtained.

1. additionthen add
2. customLeave for 4 hours
3. temperaturethen heat
4. temperatureunder reflux for 1 hour
5. customEvaporate to dryness
6. customformed in water
7. filtrationFilter the crystals
8. customformed
9. washwash them in water
10. customEvaporate the etherified filtrate to dryness
11. filtrationfilter the crystals
12. customformed
13. additionadd to
14. customthose already obtained in order
15. customto dry them