反应详情

温度

0 °C

Into a 3 L round bottom flask equipped with mechanical stirrer, thermometer and nitrogen purge was charged 2-(5-ethoxycarbonylamino-1,2,4-thiadiazol-3-yl)acetic acid (185 g, 0.80 mol, 1.0 eq.) followed by methanol (925 mL) and the resulting solution was cooled to 0° C. To the solution was bubbled in HCl gas for 30 minutes and the thinning slurry was allowed to stir overnight at 20° C. Proton NMR analysis shows complete conversion to the title compound. The solvent was removed by rotary evaporation to 400 mL and then cooled to 0° C. and seeded with pure title compound. The thickening reaction mixture was stirred at 0° C. for two hours and the white solid was collected by vacuum filtration. The solid was dried under high vacuum for 12 hours at 20° C. to give 172.2 grams of the title compound as an off white solid. 1H NMR (CD3OD): δ 1.47 (t, 3H); 3.83 (s, 3H); 3.97 (s, 2H); 4.45 (q, 2H).

1. customInto a 3 L round bottom flask equipped with mechanical stirrer
2. customthermometer and nitrogen purge
3. customTo the solution was bubbled in HCl gas for 30 minutes
4. customThe solvent was removed by rotary evaporation to 400 mL
5. temperaturecooled to 0° C.
6. customThe thickening reaction mixture
7. stirringwas stirred at 0° C. for two hours
8. filtrationthe white solid was collected by vacuum filtration
9. customThe solid was dried under high vacuum for 12 hours at 20° C.