反应详情

温度

80 °C

126 mmol of thioacetamide was dissolved in 378 ml of tetrahydrofuran, then a solution, in which 120 mmol of 2-chloroaceto acetate was dissolved in 36 ml of tetrahydrofuran, was gradually dropped with keeping a temperature at 0 to 10° C. using an ice bath. After the dropping, stirring was continued for 1 hour at a room temperature, then the temperature was heated up to 80° C. and the reaction was continued for 3 hours. The reacted liquid was kept still overnight. A recrystallized solid was filtrated, and dissolved in 50 ml of water. Sodium hydrogen carbonate was added until the pH of the solution reached 8 to 9, the product was extracted and separated into an organic layer using ethyl acetate, then dried under sodium sulfate and the solvent was evaporated out, obtaining ethyl 2,4-dimethyl-1,3-thiazole-5-carboxylate.

1. additionwas gradually dropped
2. customat 0 to 10° C.
3. waitthe reaction was continued for 3 hours
4. waitThe reacted liquid was kept still overnight
5. filtrationA recrystallized solid was filtrated
6. dissolutiondissolved in 50 ml of water
7. additionSodium hydrogen carbonate was added until the pH of the solution
8. extractionthe product was extracted
9. customseparated into an organic layer
10. customdried under sodium sulfate
11. customthe solvent was evaporated out