反应详情

3-Iodo-4-methylbenzoic acid (2.62 g, 10 mmol) was refluxed in SOCl2 (10 mL) for 1 h. The volatile components were removed on a rotavap and the residue was dissolved in benzene (10 mL), concentrated to dryness on a rotavap and further dried under vacuum. The resulting acyl chloride was added to a solution 3-(4-methyl-1H-imidazol-1-yl)-5-(trifluoromethyl)benzenamine (2.46 g, 10.2 mmol), N,N-diisopropylethylamine (1.56 g, 12 mmol), and a catalytic amount of DMAP in THF (20 mL). After stirring at rt for 2 h, the reaction was quenched with water. EtOAc was added and the layers separated. The combined organic layers were concentrated to dryness and used without purification in next step.

1. customThe volatile components were removed on a rotavap
2. dissolutionthe residue was dissolved in benzene (10 mL)
3. concentrationconcentrated to dryness on a rotavap
4. customfurther dried under vacuum
5. customthe reaction was quenched with water
6. additionEtOAc was added
7. customthe layers separated
8. concentrationThe combined organic layers were concentrated to dryness
9. customused without purification in next step