反応 #91144

反応方程式

2-Mercapto-nicotinic acid

NaH

Bromo-cyclobutane

→

title compound

2-cyclobutylsulfanyl-nicotinic acid

溶媒

DMF

反応条件

後処理

1. 1
   温度the 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
   その他After the termination of the reaction
5. 5
   濃縮the reactant was concentrated under reduced pressure
6. 6
   workup.ADDITIONThe residue was diluted with water
7. 7
   抽出The solution was extracted with EtOAc
8. 8
   乾燥The organic layer was dried with MgSO4
9. 9
   濃縮concentrated under reduced pressure

実験手順

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.

出典