반응 #2487419

반응 방정식

N-[1-(ethylsulfanyl)ethylidene]aniline

nicotinic acid hydrazide

→

3-Methyl-4-phenyl-5-(3-pyridyl)-4H-1,2,4-triazole

수율 42.0%

용매

1-butanol

반응 조건

후처리

1. 1
   기타First, into a 100-mL three-neck flask were placed
2. 2
   농축After the stirring, this reaction solution was concentrated under reduced pressure
3. 3
   기타to give an oily substance
4. 4
   세척This oily substance was washed with ethyl acetate
5. 5
   여과subjected to suction filtration
6. 6
   기타to give a solid
7. 7
   기타This solid was purified by alumina column chromatography
8. 8
   농축The obtained fraction was concentrated
9. 9
   기타to give a solid
10. 10
    세척This solid was washed with a mixed solvent of ethyl acetate and hexane, so that 3-methyl-4-phenyl-5-(3-pyridyl)-4H-1,2,4-triazole (abbreviation: HMpytz)
11. 11
    기타was obtained (a white solid, 42% yield)
12. 12
    기타The synthesis scheme of Step 1

실험 절차

First, into a 100-mL three-neck flask were placed 3.64 g of N-[1-(ethylsulfanyl)ethylidene]aniline, 20 mL of 1-butanol, and 2.78 g of nicotinic acid hydrazide, and the mixture was stirred at 130° C. for 22 hours. After the stirring, this reaction solution was concentrated under reduced pressure to give an oily substance. This oily substance was washed with ethyl acetate, and subjected to suction filtration to give a solid. This solid was purified by alumina column chromatography using ethyl acetate as a developing solvent. The obtained fraction was concentrated to give a solid. This solid was washed with a mixed solvent of ethyl acetate and hexane, so that 3-methyl-4-phenyl-5-(3-pyridyl)-4H-1,2,4-triazole (abbreviation: HMpytz) was obtained (a white solid, 42% yield). The synthesis scheme of Step 1 is illustrated in the following (a-1).

출처