反应详情

A mixture of 1-(2-methoxyphenyl)-4-[2-(2-aminobenzoyl)-aminoethyl]piperazine (3.54 g) and triethylamine (2.2 g) was dissolved in methylene chloride (50 ml), and the resulting solution was added dropwise to a solution of trichloromethyl chloroformate (0.989 g) in methylene chloride (20 ml) under stirring at between -5° and 5° C. Then, the mixture was gradually heated to room temperature at which it was held for 1 to 2 hours to effect reaction. After completion of the reaction, saturated aqueous sodium hydrogencarbonate was added to the reaction mixture and the resulting mixture was extracted with methylene chloride, the methylene chloride layer was washed with water twice and dried on anhydrous magnesium sulfate. The solvent was concentrated under vacuum and isopropanol was added to the residue to give 2.28 g of crystalline 3-[2-[4-(2-methoxyphenyl)-1-piperazinyl]-ethyl]-2,4-(1H,3H)quinazolinedione having a melting point of 217°-218° C. (recrystallized from chloroform-ether).

1. customreaction
2. additionwas added to the reaction mixture
3. extractionthe resulting mixture was extracted with methylene chloride
4. washthe methylene chloride layer was washed with water twice
5. dry with materialdried on anhydrous magnesium sulfate
6. concentrationThe solvent was concentrated under vacuum and isopropanol
7. additionwas added to the residue