反应详情

To 13.51 g of methyl 4-(2-cyclohexyl-1H-imidazol-1-yl)-2-methoxy-5-nitrobenzoate as synthesized in above Production Example 27, acetic acid 55 mL and water 55 mL were added and heated to form a solution, to which 22.59 g of 87% sodium hyposulfite was added little by little, followed by heating under reflux for 3.2 hours. The reaction liquid was cooled with ice, to which ethyl acetate and tetrahydrofuran were added, and it was rendered weakly alkaline by addition of 25% aqueous ammonia little by little. The organic layer was separated, washed with saturated brine, dried over magnesium sulfate and removed of the solvent by distillation to provide 9.13 g of the title compound.

1. additionwere added
2. temperatureheated
3. customto form a solution
4. temperatureby heating
5. temperatureunder reflux for 3.2 hours
6. customThe reaction liquid
7. additionwere added
8. customThe organic layer was separated
9. washwashed with saturated brine
10. dry with materialdried over magnesium sulfate
11. customremoved of the solvent by distillation