反应详情

A solution of (benzo[d][1,3]dioxol-7-yl)methanol (2.0 g, 13.1 mmol) and di(1H-imidazol-1-yl)methanone (4.26 g, 26.2 mmol) in 20 mL CH2Cl2 was heated overnight at 50° C. The reaction was quenched with water and extracted with CH2Cl2, and the combined layers were dried over MgSO4, filtered, and concentrated. Purification via silica gel chromatography using 10-70% EtOAc in CH2Cl2 gave (benzo[d][1,3]dioxol-7-yl)methyl 1H-imidazole-1-carboxylate (2.8 g, 86%). 1H NMR (400 MHz, CDCl3) δ 8.15 (t, J=0.9 Hz, 1H), 7.44 (t, J=1.4 Hz, 1H), 7.07 (dd, J=1.6, 0.8 Hz, 1H), 6.95 (m, 2H), 6.84 (m, 1H), 6.01 (s, 2H), 5.33 (s, 2H).

1. customThe reaction was quenched with water
2. extractionextracted with CH2Cl2
3. dry with materialthe combined layers were dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customPurification via silica gel chromatography