反应详情

2.4 g (0.056 mol) of sodium hydroxide was dissolved in 24 ml of water. 3.6 g (0.017 mol) of aminoacetonitrile sulfate was added to the solution. 30 ml of ether containing 3.0 g (0.017 mol) of 2-fluoroisonicotinoyl chloride was added dropwise to the solution while the temperature was kept below 5° C. The mixture was stirred at room temperature for 2 h to conduct a reaction. Water and ethyl acetate were added to the mixture to conduct extraction. The organic layer was washed with a saturated aqueous common salt solution and dried over anhydrous sodium sulfate. The solvent was distilled. The resulting crude crystalls were recrystallized from a solvent mixture of n-hexane and ethyl acetate to obtain 2.3 g (yield: 75.3%) of white crystal having a melting point of 124° to 125° C.

1. customwas kept below 5° C
2. customa reaction
3. extractionextraction
4. washThe organic layer was washed with a saturated aqueous common salt solution
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThe solvent was distilled
7. customThe resulting crude crystalls were recrystallized from a solvent mixture of n-hexane and ethyl acetate