反应详情

To a suspension of lithium aluminium hydride (3.78 g) in tetrahydrofuran (150 ml) was added 5-amino-1-methyl-N-[2-(tritylamino)ethyl]-1H-pyrazole-4-carboxamide (10.64 g) at room temperature. The mixture was stirred under reflux for 18 hours. After cooling on an ice bath, to the reaction mixture were added sodium fluoride (20 g) and aqueous tetrahydrofuran solution (10 ml). The insoluble materials were removed by filtration. The resulting filtrate was concentrated in vacuo, and the residue was dissolved in chloroform. The solution was washed with 10% aqueous sodium hydroxide solution. The organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The oily residue was triturated with ethyl acetate and dried in vacuo to give N-[(5-amino-1-methyl-1H-pyrazol-4-yl)methyl]-N′-tritylethane-1,2-diamine (3.2 g) as a solid.

1. temperatureunder reflux for 18 hours
2. temperatureAfter cooling on an ice bath, to the reaction mixture
3. customThe insoluble materials were removed by filtration
4. concentrationThe resulting filtrate was concentrated in vacuo
5. dissolutionthe residue was dissolved in chloroform
6. washThe solution was washed with 10% aqueous sodium hydroxide solution
7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
8. filtrationfiltered
9. concentrationconcentrated in vacuo
10. customThe oily residue was triturated with ethyl acetate
11. customdried in vacuo