反应详情

A mixture of 8 g (0.026 mol) of ethyl 4,5-diphenyl-1H-pyrazole-1-acetate of example 1 and 40 mL (0.25 mol) of diethylaminopropylamine was heated on a steam bath under nitrogen for 14 hours. The excess diethylaminopropylamine was stripped in vacuo and the residue dissolved in ether. The ether solution was washed two times with water, once with saturated sodium chloride, dried over magnesium sulfate, filtered and evaporated in vacuo. The resulting white residue was dissolved in ether and a small amount of undesired material was removed by filtration after addition of some pentane. The filtrate was stripped, redissolved in ether, dried over magnesium sulfate, treated with decolorizing carbon, filtered and evaporated. The resulting residue was triturated in water filtered and rinsed with water to yield 8.55 g (82%) of N-[3-(diethylamino)propyl]-4,5-diphenyl-1H-pyrazole-1-acetamide hemihydrate, mp 70°-74° C. The product can be recrystallized from wet ether.

1. temperaturewas heated on a steam bath under nitrogen for 14 hours
2. washThe ether solution was washed two times with water
3. dry with materialonce with saturated sodium chloride, dried over magnesium sulfate
4. filtrationfiltered
5. customevaporated in vacuo
6. dissolutionThe resulting white residue was dissolved in ether
7. customa small amount of undesired material was removed by filtration
8. additionafter addition of some pentane
9. dissolutionredissolved in ether
10. dry with materialdried over magnesium sulfate
11. additiontreated with decolorizing carbon
12. filtrationfiltered
13. customevaporated
14. customThe resulting residue was triturated in water
15. filtrationfiltered
16. washrinsed with water