반응 #91126

반응 방정식

2-Chloro-6-methyl-nicotinic acid methyl ester

2-chloro-6-methyl-nicotinic acid methyl ester

Cs2CO3

propane-2-thiol

→

title compound

수율 69.8%

2-isopropylsulfanyl-6-methyl-nicotinic acid methyl ester

수율 69.8%

용매

DMF

반응 조건

후처리

1. 1
   농축The reactant was concentrated under reduced pressure
2. 2
   기타to remove the solvent
3. 3
   workup.ADDITIONThe residue was added with water
4. 4
   추출extracted with EtOAc
5. 5
   건조The organic layer was dried with MgSO4
6. 6
   여과filtered
7. 7
   농축concentrated under reduced pressure
8. 8
   기타The obtained residue was purified by column chromatography (eluent EtOAc/Hex=1/5)

실험 절차

2-Chloro-6-methyl-nicotinic acid methyl ester (1.39 g, 7.44 mmol) obtained in Step A was dissolved in DMF (15 mL). Cs2CO3(4.88 g, 14.99 mmol) and propane-2-thiol (1.39 mL, 14.99 mmol) were added to the solution, and the mixture was stirred at room temperature for 2 hours. The reactant was concentrated under reduced pressure to remove the solvent. The residue was added with water and then extracted with EtOAc. The organic layer was dried with MgSO4, filtered and concentrated under reduced pressure. The obtained residue was purified by column chromatography (eluent EtOAc/Hex=1/5) to obtain the title compound (1.17 g, 69%).

출처