反応 #1687639

反応方程式

2-(ethylthio) ethanol

MeSO3H

3-(4-(2-ethylthio-1-ethoxy)- 1,2,5-thiadiazol-3-yl)pyridine

NaOH

water

→

1,2,5,6-tetrahydro-1-methyl-3-(3-(2-ethylsulfinyl-1-ethoxy)- 1,2,5-thiadiazol-4-yl)pyridine oxalate

反応条件

後処理

1. 1
   その他After a reaction time of 3.5 h.
2. 2
   抽出extracted with ethyl acetate
3. 3
   乾燥The combined extracts were dried over MgSO4
4. 4
   その他evaporated under vacuum

実験手順

1,2,5,6-tetrahydro-1-methyl-3-(3-(2-ethylsulfinyl-1-ethoxy)- 1,2,5-thiadiazol-4-yl)pyridine oxalate was prepared in the same manner using 2-(ethylthio) ethanol as the starting alcohol. The intermediate 3-(4-(2-ethylthio-1-ethoxy)- 1,2,5-thiadiazol-3-yl)pyridine was oxidized with 1.1 equivalent of NaIO4 and 1 equivalent MeSO3H using water as the reaction solvent. After a reaction time of 3.5 h. the solution was made basic with 2N NaOH and extracted with ethyl acetate. The combined extracts were dried over MgSO4 and evaporated under vacuum. The resulting sulfoxide was then converted to the title compound in the same manner described above. M.p. 171°-172° C., M+ : 302. Compound 45.

出典