반응 #91144

반응 방정식

2-Mercapto-nicotinic acid

NaH

Bromo-cyclobutane

→

title compound

2-cyclobutylsulfanyl-nicotinic acid

용매

DMF

반응 조건

후처리

1. 1
   온도the solution was cooled to 0˜5° C
2. 2
   workup.STIRRINGthe mixture was stirred at 55˜65° C. for 3 hours
3. 3
   workup.STIRRINGstirred at room temperature for 12 hours
4. 4
   기타After the termination of the reaction
5. 5
   농축the reactant was concentrated under reduced pressure
6. 6
   workup.ADDITIONThe residue was diluted with water
7. 7
   추출The solution was extracted with EtOAc
8. 8
   건조The organic layer was dried with MgSO4
9. 9
   농축concentrated under reduced pressure

실험 절차

2-Mercapto-nicotinic acid (0.1 g, 0.64 mmol) was dissolved in DMF (2 mL), and the solution was cooled to 0˜5° C. NaH (0.13 g, 3.2 mmol) was added slowly thereto, and the mixture was stirred at 0˜5° C. for 30 minutes. Bromo-cyclobutane (0.12 mL, 1.28 mmol) was added thereto, and the mixture was stirred at 55˜65° C. for 3 hours, and then stirred at room temperature for 12 hours. After the termination of the reaction, the reactant was concentrated under reduced pressure. The residue was diluted with water, and then 3N HCl was used to adjust the pH of the solution to 2˜3. The solution was extracted with EtOAc. The organic layer was dried with MgSO4 and concentrated under reduced pressure to obtain the title compound, which was used in the next step without a separate purification process.

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