تفاعل #2487419

معادلة التفاعل

N-[1-(ethylsulfanyl)ethylidene]aniline

nicotinic acid hydrazide

→

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

المردود 42.0%

المذيبات

1-butanol

ظروف التفاعل

المعالجة

1. 1
   أخرىFirst, into a 100-mL three-neck flask were placed
2. 2
   تركيزAfter the stirring, this reaction solution was concentrated under reduced pressure
3. 3
   أخرىto give an oily substance
4. 4
   غسيلThis oily substance was washed with ethyl acetate
5. 5
   ترشيحsubjected to suction filtration
6. 6
   أخرىto give a solid
7. 7
   أخرىThis solid was purified by alumina column chromatography
8. 8
   تركيزThe obtained fraction was concentrated
9. 9
   أخرىto give a solid
10. 10
    غسيلThis 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
    أخرىwas obtained (a white solid, 42% yield)
12. 12
    أخرىThe synthesis scheme of Step 1

الإجراء التجريبي

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).

المصدر