反应详情

Aluminium chloride (80 mmol), dissolved in 200 ml of anhydrous ether, is added to a suspension of lithium aluminium hydride at 0° C. in 300 ml of anhydrous ether. After stirring for 10 minutes, the compound obtained in Step A (20 mmol), dissolved in 200 ml of anhydrous ether, is added. After 30 minutes, the mixture is hydrolysed, with caution and in the cold state, using sodium hydroxide solution (10 g; 40 ml). The precipitate formed is then filtered off and washed with copious amounts of ether. The residue obtained after evaporation is taken up in water and the aqueous phase is extracted with dichloromethane. The organic phase is then washed with water, dried and decoloured, and is then treated with gaseous hydrogen chloride and evaporated. The oil obtained is precipitated from ethyl acetate, and the precipitate formed is filtered off under suction and then recrystallised to yield the title product in the form of a white solid.

1. additionis added
2. waitAfter 30 minutes
3. customThe precipitate formed
4. filtrationis then filtered off
5. washwashed with copious amounts of ether
6. customThe residue obtained
7. customafter evaporation
8. extractionthe aqueous phase is extracted with dichloromethane
9. washThe organic phase is then washed with water
10. customdried
11. additionis then treated with gaseous hydrogen chloride
12. customevaporated
13. customThe oil obtained
14. customis precipitated from ethyl acetate
15. customthe precipitate formed
16. filtrationis filtered off under suction
17. customrecrystallised