反应详情

温度

60 °C

5-(2-Methoxy-ethyl)-4-methyl-thiophene-2-sulfonic acid amide (0.1556 g, 0.661 mmol) was dissolved in 4 mL of abs. acetonitrile and treated successively with phenyl chloroformate (0.103 g, 1.00 eq.) and triethylamine (0.229 mL, 2.5 eq.), and the mixture kept at ambient temperature for 1 h. The above prepared 5-ethyl-4-methyl-thiazol-2-ylamine (0.094 g, 1.00 eq.), dissolved in a tiny amount of acetonitrile, was then added, and the mixture heated to 60° C. over night. Cooling, pouring onto crashed ice/NH4Cl, twofold extraction with ethyl acetate, washing with brine, drying over magnesium sulfate, and evaporation of the solvents, followed by flash chromatography (SiO2, ethyl acetate), yielded eventually 0.089 g of the title compound as light brown solid.

1. additionwas then added
2. temperatureCooling
3. additionpouring
4. extractionice/NH4Cl, twofold extraction with ethyl acetate
5. washwashing with brine
6. dry with materialdrying over magnesium sulfate, and evaporation of the solvents