反应详情

2-Mercaptonicotinic acid (90 g, 0.58 mol) was suspended in N,N-dimethylformamide (660 mL), and carbonyldiimidazole (110 g, 0.70 mol) was added thereto under ice-cooling, and then the mixture was stirred at room temperature for 2 hours. Water (5.4 mL) was added thereto, the whole was stirred for 40 minutes. 3,5-Xylidine (76 mL, 0.61 mol) was added thereto, and the mixture was stirred for 16 hours at 60° C. The mixture was allowed to stand, water (1.3 L) was added thereto, and then the precipitated solid was filtered off. The solid was dried under reduced pressure at 45° C. to give 130 g of the title reference compound as a yellow solid. (Yield 89%)

1. temperatureunder ice-cooling
2. stirringthe whole was stirred for 40 minutes
3. stirringthe mixture was stirred for 16 hours at 60° C
4. filtrationthe precipitated solid was filtered off
5. customThe solid was dried under reduced pressure at 45° C.
6. customto give 130 g of the title reference compound as a yellow solid