反应详情

温度

80 °C

Into a 50-mL round-bottom flask, was placed a solution of methyl 3-(4-chloro-2-(methoxymethyl)-1H-imidazol-5-yl)-4-methylbenzoate (compound 27.4, 380 mg, 1.29 mmol, 1.00 equiv) in HBr (40% in AcOH) (10 mL). The solution was stirred overnight at 80° C., then cooled and concentrated under reduced pressure. The crude residue was purified by prep-HPLC (WATER WITH 0.05% TFA and CH3CN (0% CH3CN in 3 min, then up to 100% for 5 min, down to 0% in 1 min); Detector, 254 & 220 nm. The fractions containing clean product were combined and lyophilized to yield 171 mg (50%) of the title compound as yellow crude oil.

1. customInto a 50-mL round-bottom flask, was placed
2. temperaturecooled
3. concentrationconcentrated under reduced pressure
4. customThe crude residue was purified by prep-HPLC (WATER WITH 0.05% TFA and CH3CN (0% CH3CN in 3 min
5. waitup to 100% for 5 min
6. waitdown to 0% in 1 min)
7. additionThe fractions containing clean product