反应详情

温度

5 °C

1-(3,4-Dichloro-phenyl)-1H-imidazole-4-carboxylic acid (20.0 g, 77.8 mmol) was treated with 1M BH3 THF complex (100 ml) and refluxed for 2 h. The mixture was cooled to 5° C. and MeOH (20 ml) was added slowly. After evaporation of all volatiles the residue was taken up in 2N HCl solution (100 ml) and refluxed for 2 h. After filtration the hot aqueous phase was slowly treated with 2N NaOH solution until pH 10. On cooling the title compound crystallizes as a white material (12.2 g, 65%). Mp. 146-147° C. (H2O), MS: m/e=242 (M+).

1. temperaturerefluxed for 2 h
2. customAfter evaporation of all volatiles the residue
3. temperaturerefluxed for 2 h
4. filtrationAfter filtration the hot aqueous phase
5. additionwas slowly treated with 2N NaOH solution until pH 10
6. temperatureOn cooling the title compound
7. customcrystallizes as a white material (12.2 g, 65%)