反应详情

To a solution of ethyl 2-mercapto-1,3-thiazole-4-carboxylate ((Ref: J. Am. Chem. Soc. 1935, 57, 1127), 0.694 g, 3.67 mmol) in Et2O (40 mL) at 0° C. was added EtMgBr (3 M in Et2O, 2.7 mL, 8.07 mmol). The reaction mixture was heated to reflux for 15 min, quenched with NH4Cl, extracted with 3 portions of Et2O, dried over MgSO4, filtered and concentrated in vacuo. The crude material was treated with more EtMgBr (3 M in Et2O, 6 mL, 18 mmol) at rt for 10 min, quenched, extracted and isolated in the same way. The residue was washed with Et2O and Et2O/hexane to afford the title compound.

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 15 min
3. customquenched with NH4Cl
4. extractionextracted with 3 portions of Et2O
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customquenched
9. extractionextracted
10. customisolated in the same way
11. washThe residue was washed with Et2O and Et2O/hexane