反应详情

2-Ethoxy-N-(4-methyl-2-propylimidazol-1-yl)benzamide from Example D (3.5 g, 12.2 mmol) is dissolved in 480 ml of a dioxane/water mixture, and sodium carbonate (3.9 g, 36.6 mmol) and iodine (6.8 g, 26.8 mmol) are added. The mixture is stirred with exclusion of light at room temperature for 24 hours. 50 ml of ethyl acetate are added to the reaction mixture and washed twice with 50 ml of saturated sodium sulphite solution each time. The combined aqueous phases are re-extracted twice with 50 ml of ethyl acetate each time, and the combined organic phase is dried with sodium sulphate and concentrated in a rotary evaporator.

1. washwashed twice with 50 ml of saturated sodium sulphite solution each time
2. extractionThe combined aqueous phases are re-extracted twice with 50 ml of ethyl acetate each time
3. dry with materialthe combined organic phase is dried with sodium sulphate
4. concentrationconcentrated in a rotary evaporator