反应 #2487419

反应方程式

N-[1-(ethylsulfanyl)ethylidene]aniline

nicotinic acid hydrazide

→

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

收率 42.0%

溶剂

1-butanol

反应条件

后处理

1. 1
   其他First, into a 100-mL three-neck flask were placed
2. 2
   浓缩After the stirring, this reaction solution was concentrated under reduced pressure
3. 3
   其他to give an oily substance
4. 4
   洗涤This oily substance was washed with ethyl acetate
5. 5
   过滤subjected to suction filtration
6. 6
   其他to give a solid
7. 7
   其他This solid was purified by alumina column chromatography
8. 8
   浓缩The obtained fraction was concentrated
9. 9
   其他to give a solid
10. 10
    洗涤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)
11. 11
    其他was obtained (a white solid, 42% yield)
12. 12
    其他The synthesis scheme of Step 1

实验过程

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).

来源