反应详情

温度

25 °C

To the solution of 1.18 g of 1-(-4-bromo-1-methyl-1H-imidazol-2-yl)-2,2,2-trichloroethanone in 10 mL of methanol was added 42 mg of sodium methoxide and the resulting mixture was stirred at 25° C. for 20 min. TLC showed completion of the reaction. The solution was evaporated, redissolved in 30 mL of DCM, washed with water (15 mL×2) and brine (15 mL). The solution was dried over anhydrous sodium sulfate and filtered. The residue was purified by silica gel column (DCM/MeOH=60/1) to give 4-bromo-1-methyl-1H-imidazole-2-carboxylic acid methyl ester (0.575 g, yield 68%). 1H NMR (300 MHz, CDCl3) δ 7.02 (s, 1H), 4.00 (s, 3H). 3.93 (s, 3H). LC-MS calcd for C6H7BrN2O2 (m/e) 217.97, obsd 219 and 221 [M+1]+

1. customcompletion of the reaction
2. customThe solution was evaporated
3. dissolutionredissolved in 30 mL of DCM
4. washwashed with water (15 mL×2) and brine (15 mL)
5. dry with materialThe solution was dried over anhydrous sodium sulfate
6. filtrationfiltered
7. customThe residue was purified by silica gel column (DCM/MeOH=60/1)