反应详情

To a suspension of lithium aluminum hydride (5.41 g) in tetrahydrofuran (200 ml) was added a solution of 4-[(E)-2-cyanoethenyl]-1-[2-(trityloxy)ethyl]-5-aminopyrazole (15 g) in tetrahydrofuran (100 ml) under ice-cooling. The mixture was refluxed for 3.5 hours. After cooling on an ice bath, sodium fluoride (24 g) and water (10.3 ml) were added to the reaction mixture. The insoluble materials were removed by filtration. The filtrate was concentrated in vacuo to give 4-(3-aminopropyl)-1-(2-triphenylmethyloxyethyl)-5-aminopyrazole (13.7 g). This product was used in the next step without further purification.

1. temperaturecooling
2. temperatureThe mixture was refluxed for 3.5 hours
3. temperatureAfter cooling on an ice bath
4. customThe insoluble materials were removed by filtration
5. concentrationThe filtrate was concentrated in vacuo