反应详情

Ethyl 5-methyl-4-1H-imidazolecarboxylate (6.16 g) in toluene (100 ml), triphenylmethyl chloride (11.12 g) and triethylamine (5.6 ml) were heated at reflux for 18 h. Toluene was removed under reduced pressure and the residue was dissolved in dichloromethane (100 ml), washed with water (4×50 ml) dried (MgSO4) and evaporated. The residue was purified by column chromatography on silica using 1% methanol in dichloromethane as eluant with a trace of triethylamine. This afforded the title compound (11 g), m.p. 188°-190° C. δH (250 MHz, CDCl3) 1.38-1.42 (3 H, t, J=6.5 Hz, CH3), 1.86 (3 H, s, CH3), 4.36-4.40 (2 H, q, J=7.2 Hz, CH2), 7.10-7.46 (16 H, m, ArH); m/z (NoM+), 243 (Ph3C+, 100%).

1. temperatureat reflux for 18 h
2. customToluene was removed under reduced pressure
3. dissolutionthe residue was dissolved in dichloromethane (100 ml)
4. washwashed with water (4×50 ml)
5. dry with materialdried (MgSO4)
6. customevaporated
7. customThe residue was purified by column chromatography on silica using 1% methanol in dichloromethane as eluant with a trace of triethylamine