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 and the mixture was stirred at room temperature for 1 h and then cooled to 5° C. or below. A liquid mixture of 3.0 g (0.017 mol) of 2-chloroisonicotinoyl chloride and 30 ml of ether was added dropwise thereto at 5° C. or below lest unfavorable heat generation should occur. The mixture was then stirred at room temperature for 2 h to conduct a reaction. Water and ethyl acetate were added thereto to conduct extraction. The extract was washed with a saturated aqueous common salt solution, dried over anhydrous sodium sulfate and concentrated. The resulting crystals were recrystallized from a liquid mixture of n-hexane and ethyl acetate to obtain 2.7 g (yield: 81.2%) of the intended product as white crystals having a melting point of 131° to 132° C.

1. temperaturecooled to 5° C. or below
2. additionwas added dropwise
3. customat 5° C. or below
4. stirringThe mixture was then stirred at room temperature for 2 h
5. customa reaction
6. extractionextraction
7. washThe extract was washed with a saturated aqueous common salt solution
8. dry with materialdried over anhydrous sodium sulfate
9. concentrationconcentrated
10. customThe resulting crystals were recrystallized from a liquid mixture of n-hexane and ethyl acetate