反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
1-(2-Fluoro-4-nitro-phenyl)-4-methyl-1H-imidazole (4.66 g, 21.1 mmol) was dissolved in a mixture of methanol (25 mL) and tetrahydrofuran (100 mL). The solution was cooled to 0° C. under an atmosphere of nitrogen. Ammonium formiate (6.64 g, 105 mmol) and 10% palladium on charcoal (0.24 g) were added and the mixture was stirred at ambient temperature for 18 hours. It was filtered through celite. The celite was washed with methanol and the filtrate was evaporated under reduced pressure to dryness. The residue was partitioned between ethyl acetate and 10% aqueous sodium bicarbonate solution. The organic layer was separated, washed with brine, dried over sodium sulfate and the solvent was evaporated under reduced pressure to yield the title compound (3.89 g, 97%) as a yellow solid. 1H NMR (DMSO-D6, 300 MHz): δ (ppm)=7.62 (s, 1H), 7.12 (t, 1H), 7.01 (s, 1H), 6.41-6.51 (m, 2H), 5.64 (br s, 2H), 2.13 (s, 3H).
WORKUP
后处理
- filtrationIt was filtered through celite
- washThe celite was washed with methanol
- customthe filtrate was evaporated under reduced pressure to dryness
- customThe residue was partitioned between ethyl acetate and 10% aqueous sodium bicarbonate solution
- customThe organic layer was separated
- washwashed with brine
- dry with materialdried over sodium sulfate
- customthe solvent was evaporated under reduced pressure