反应详情

温度

35 °C

A mixture of 11.7 g of 4-imidazolecarboxylic acid, 18.7 g of 1,1'-carbonyldiimidazole, 20 ml of diisopropylethylamine and 600 ml of DMF was heated at 35° C. for approximately 18 hours. Twenty milliters of aminodiphenylmethane were added and the solution stirred at 35° C. for approximately 21/2 days. The mixture was concentrated in vacuo and the residue added to 400 ml of water. The mixture was extracted with ethyl acetate and the organic layer was washed with a saturated sodium chloride solution, dried over magnesium sulfate, and concentrated in vacuo. Two crystallizations from hot ethyl acetate/hexane provided 11 grams of the desired titled intermediate, m.p. 201°-202° C.

1. concentrationThe mixture was concentrated in vacuo
2. additionthe residue added to 400 ml of water
3. extractionThe mixture was extracted with ethyl acetate
4. washthe organic layer was washed with a saturated sodium chloride solution
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. customTwo crystallizations from hot ethyl acetate/hexane