反应详情

温度

0 °C

2.2 g (10.0 mmol) of the compound from Example 2A are initially charged in 50 ml of ethanol. 2.1 g (10.0 mmol) of the compound from Example 15A and 380 mg (2.0 mmol) of p-toluenesulfonic acid are added, and the mixture is stirred under reflux for 16 h. The mixture is then cooled to 0° C., and the solid formed is filtered off and washed once with a little ethanol (batch 1). The mother liquor is concentrated and the residue is triturated with a little ethanol. The solid obtained is filtered off and washed once with ethanol (batch 2). The two solids batches are combined and dried under high vacuum. The solid is then stirred in tert-butyl methyl ether for 30 min, filtered off again and dried under high vacuum.

1. temperatureunder reflux for 16 h
2. customthe solid formed
3. filtrationis filtered off
4. washwashed once with a little ethanol (batch 1)
5. concentrationThe mother liquor is concentrated
6. customthe residue is triturated with a little ethanol
7. customThe solid obtained
8. filtrationis filtered off
9. washwashed once with ethanol (batch 2)
10. customdried under high vacuum
11. stirringThe solid is then stirred in tert-butyl methyl ether for 30 min
12. filtrationfiltered off again
13. customdried under high vacuum