反应详情

Into a flask containing a solution of methyl 2-(hydroxymethyl)-1-((2-(tri-methylsilyl)-ethoxy)methyl)-1H-imidazole-4-carboxylate (1 g, 3.49 mmol) in DMF (25 ml), imidazole (0.490 g, 6.91 mmol), catalytic DMAP and TBDMSCl (0.790 g, 5.27 mmol) were added. The resulting mixture was stirred at RT for 12 h. The reaction mixture was quenched with saturated aqueous solution of NaHCO3 and extracted with EtOAc. The organic layer was concentrated and purified by flash column chromatography. Yield 800 mg. 1H-NMR (400 MHz; DMSO-d6): δ −0.04 (s, 9H), 0.05 (s, 6H), 0.80 (t, 2H), 0.86 (s, 9H), 3.49 (t, 2H), 3.74 (s, 3H), 4.71 (s, 2H), 5.41 (s, 2H), 8.02 (s, 1H). LC-MS: [M+1]=401.10.

1. additionwere added
2. customThe reaction mixture was quenched with saturated aqueous solution of NaHCO3
3. extractionextracted with EtOAc
4. concentrationThe organic layer was concentrated
5. custompurified by flash column chromatography