反应详情

温度

0 °C

To a mixture of 1.37 g (5 mmol) of 4-[(2-methylbenzoyl)amino]benzoyl chloride in 15 ml of methylene chloride, cooled to 0° C. is added 1.5 ml of triethylamine. After stirring for 3 minutes, 5 mmol of 10,11-dihydro-5H-imidazo[2,1-c][1,4]benzodiazepine in 5 ml of methylene chloride is added. The cooling bath is removed and after about 30 minutes a complete solution is obtained. The reaction mixture is allowed to stir at room temperature for 1 hour and the volatiles are concentrated in vacuo. The residue is dissolved in 100 ml of ethyl acetate and washed with water, 2N citric acid, and brine. The solution is dried with Na2 SO4 and the volatiles concentrated in vacuo to give the desired product as a solid.

1. customThe cooling bath is removed and after about 30 minutes a complete solution
2. customis obtained
3. stirringto stir at room temperature for 1 hour
4. concentrationthe volatiles are concentrated in vacuo
5. dissolutionThe residue is dissolved in 100 ml of ethyl acetate
6. washwashed with water, 2N citric acid, and brine
7. customThe solution is dried with Na2 SO4
8. concentrationthe volatiles concentrated in vacuo