反应详情

Ethyl 2-(4-methylthiazol-2-yl)acetate (1 g, 5.4 mmol, Eq: 1.00) was dissolved in DMF (5 mL). 1,2-dibromoethane (1.62 g, 744 μL, 8.64 mmol, Eq: 1.60) and Cs2CO3 (4.4 g, 13.5 mmol, Eq: 2.50) were added. The reaction mixture was stirred 48 h at RT. The reaction mixture was poured into 0.5 M aqueous HCl (100 mL) and extracted with EtOAc (3×50 mL). The combined organic layers were dried over Na2SO4, filtered and evaporated. The crude material was purified by flash chromatography (silica gel, 50 g, 0% to 50% EtOAc in heptane) to yield 1.14 g (73.6%) of a light yellow liquid. MS (ESI): m/z=212.0 [M+H]+.

1. extractionextracted with EtOAc (3×50 mL)
2. dry with materialThe combined organic layers were dried over Na2SO4
3. filtrationfiltered
4. customevaporated
5. customThe crude material was purified by flash chromatography (silica gel, 50 g, 0% to 50% EtOAc in heptane)