反应详情

(3-Phenyl-1H-1,2,4-triazol-5-yl)acetic acid (0.020 g) and N,N′-carbonyl diimidazole (0.016 g) in dichloromethane was stirred under nitrogen for 3 minutes. 1-(3,4-Dichlorobenzyl)-4-piperidinamine hydrochloride (0.031 g) and triethylamine (0.036 g) was then added and allowed to stir for 1 hour under nitrogen. Saturated sodium hydrogen carbonate was added to the reaction with the resulting solution being extracted three times with dichloromethane. The pooled organic phases were washed once with water, once with brine, dried over magnesium sulfate, filtered and the solvent removed under reduced pressure to a white solid. This was purified by RPHPLC (75%-5%, 0.1% ammonium acetate/acetonitrile). Saturated sodium hydrogen carbonate was added to the pooled collected fractions with the resulting solution being extracted three times with dichloromethane. The pooled organic phases were washed once with water, once with brine, dried over magnesium sulfate, filtered and the solvent removed under reduced pressure to leave N-[1-(3,4-dichlorobenzyl)-4-piperidinyl]-2-(3-phenyl-1H-1,2,4-triazol-5-yl)acetamide(0.031 g).

1. extractionbeing extracted three times with dichloromethane
2. washThe pooled organic phases were washed once with water, once with brine
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. customthe solvent removed under reduced pressure to a white solid
6. customThis was purified by RPHPLC (75%-5%, 0.1% ammonium acetate/acetonitrile)
7. additionSaturated sodium hydrogen carbonate was added to the
8. custompooled collected fractions with the resulting solution
9. extractionbeing extracted three times with dichloromethane
10. washThe pooled organic phases were washed once with water, once with brine
11. dry with materialdried over magnesium sulfate
12. filtrationfiltered
13. customthe solvent removed under reduced pressure