反应详情

In 9 ml of N,N-dimethylformamide was dissolved 740 mg of 5-chloro-3-methylthio-1,2,4-thiadiazole, and 1.25 g of 3,5-dimethylpiperidine (a mixture of 8:2 geometrical isomers) was added dropwise under ice-cooling. The mixture was stirred at room temperature for 20 minutes. The reaction mixture was diluted with tert-butyl methyl ether, and extracted with tert-butyl methyl ether after the addition of 10% hydrochloric acid. The organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 860 mg of 3-methylthio-5-(3,5-dimethylpiperidino)-1,2,4-thiadiazole.

1. additiona mixture of 8:2 geometrical isomers)
2. additionwas added dropwise under ice-
3. temperaturecooling
4. extractionextracted with tert-butyl methyl ether
5. additionafter the addition of 10% hydrochloric acid
6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
7. concentrationconcentrated under reduced pressure