反应详情

温度

42.5 °C

To a solution of 3-iodobenzoic acid tert-butyl ester (4.6 g) in THF (20 mL) at −40° C. under N2 was added cyclohexylmagnesium chloride (2M in THF, 8.5 mL). The solution was kept at −40° C. to 0° C. for 20 min., when 3-(5-amino-4-cyano-imidazol-1-yl)-N-cyclopropyl-4-methyl-benzamide was added and the reaction was kept at rt for 1 h. Then HCl (4 M, 10 mL) was added and the mixture was heated at 40 to 45° C. overnight. The mixture was neutralized with K2CO3 solution and extracted with EtOAc (2×100 mL) and the combined organics dried over Na2SO4, and concentrated. Purification of the crude product by column chromatography (EtOAc: MeOH=6:1) gave the desired product (0.46 g).

1. waitthe reaction was kept at rt for 1 h
2. extractionextracted with EtOAc (2×100 mL)
3. dry with materialthe combined organics dried over Na2SO4
4. concentrationconcentrated
5. customPurification of the crude product by column chromatography (EtOAc: MeOH=6:1)