反应详情

25 Parts of 7-chloro-5-(o-chlorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine is dissolved in 250 parts by volume of methylene chloride. To this solution 15 parts of 2-chloroethylisocyanate is slowly added with stirring. The resultant mixture is stirred at ambient temperature for about 90 minutes. The resulting dark brown solution is filtered through a layer of activated magnesium silicate, the filtrate dried and treated with charcoal. After removal of charcoal by filtration the solvent is removed from the resultant filtrate to affort an oil. This oil is dissolved in about 100 parts by volume of ether and the resultant solution cooled to give 7-chloro-N-(2-chloroethyl)-5-(o-chlorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine-1-carboxamide as crystalline solid melting at about 150°-153° C. This compound is represented by the following formula ##STR19##

1. filtrationThe resulting dark brown solution is filtered through a layer of activated magnesium silicate
2. customthe filtrate dried
3. additiontreated with charcoal
4. customAfter removal of charcoal
5. filtrationby filtration the solvent
6. customis removed from the resultant filtrate
7. dissolutionThis oil is dissolved in about 100 parts by volume of ether
8. temperaturethe resultant solution cooled