反应详情

温度

65 °C

In an appropriate vessel, methyl 3-aminothiophene-2-carboxylate (2.5 g; 15.9 mmol) was combined with 4-tert-butylbenzene sulfonyl chloride (3.70 g; 15.9 mmol) and dissolved by addition of pyridine (5.00 mL; 63.2 mmol). The reaction mixture was heated at 65° C. for 2 hours cooled to room temperature, diluted with aqueous hydrochloric acid (100 mL; 2M) and extracted with dichloromethane (3×30 mL). The combined organic extracts were washed with aqueous hydrochloric acid (100 mL), dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The resulting crude solid was recrystallized from a minimal amount of isopropanol to give the title product as a yellow solid (5.2 g).

1. temperaturecooled to room temperature
2. extractionextracted with dichloromethane (3×30 mL)
3. washThe combined organic extracts were washed with aqueous hydrochloric acid (100 mL)
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe resulting crude solid was recrystallized from a minimal amount of isopropanol