反应详情

温度

20 °C

130 g of paspalic acid are added rapidly to 780.1 g of a 40% strength solution of tetrabutylammonium hydroxide in water, with stirring and under a stream of nitrogen. The mixture is brought to 30±2° C. and allowed to react at this temperature for 20 hours. The reaction medium is cooled to about 20° C. and held at this temperature for 3 h 30 min. 918 g of water are added, followed by acidification using 95% strength sulphuric acid until the pH is 3.5, while maintaining the temperature at about 30° C. The reaction mixture is then cooled to 10±2° C. and held at this temperature for 30 minutes. The mixture is filtered through a sinter funnel under a vacuum of 0.4 bar, washed 3 times with 300 ml of water and then dried for 14 hours at 75±2° C. and 20 mbar. This gives 107 g of lysergic acid comprising less than 3% of isolysergic acid and the RRi is 80% (RRi=weight of 100% lysergic acid isolated/weight of 100% paspalic employed).

1. customis brought to 30±2° C.
2. customto react at this temperature for 20 hours
3. temperaturewhile maintaining the temperature at about 30° C
4. temperatureThe reaction mixture is then cooled to 10±2° C.
5. waitheld at this temperature for 30 minutes
6. filtrationThe mixture is filtered through a sinter funnel under a vacuum of 0.4 bar
7. washwashed 3 times with 300 ml of water
8. customdried for 14 hours at 75±2° C.