反应详情

To a stirred solution of methyl imidazol-4-ylacetate hydrochloride from Step A (4.30 g, 24.3 mmol) in dry DMF (50 mL) under argon were added triethylamine (5.41 g, 53.5 mmol) and triphenylmethyl bromide (8.64 g, 26.7 mmol). The reaction mixture was stirred at ambient temperature overnight, then partitioned between water (250 mL) and EtOAc (250 mL). The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by flash column chromatography, eluting with 50% hexane in EtOAc to remove nonpolar impurities, then EtOAc to elute the titled product as a white solid.

1. custompartitioned between water (250 mL) and EtOAc (250 mL)
2. dry with materialThe organic layer was dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by flash column chromatography
6. washeluting with 50% hexane in EtOAc
7. customto remove nonpolar impurities
8. washEtOAc to elute the titled product as a white solid