反应详情

A solution of 1.2 g. of 4-methyl-10-(methylthio)-4H-thieno[3,4-b] [1,5] benzodiazepine in 6 ml. of N-methylpiperazine is treated with 2-3 drops of glacial acetic acid and heated under reflux for 4 days. The solution is concentrated to dryness and the residue is warmed with dilute acetic acid. The acidic solution is filtered, cooled, and made alkaline with concentrated ammonium hydroxide solution. The precipitate is collected, washed with water and dissolved in chloroform. The chloroform solution is dried and concentrated to an oil, which slowly crystallizes. Recrystallization from ethanol gives yellow crystals, m.p. 83°-85°C.

1. temperatureheated
2. temperatureunder reflux for 4 days
3. concentrationThe solution is concentrated to dryness
4. temperaturethe residue is warmed with dilute acetic acid
5. filtrationThe acidic solution is filtered
6. temperaturecooled
7. customThe precipitate is collected
8. washwashed with water
9. dissolutiondissolved in chloroform
10. dry with materialThe chloroform solution is dried
11. concentrationconcentrated to an oil, which
12. customslowly crystallizes
13. customRecrystallization from ethanol
14. customgives yellow crystals, m.p. 83°-85°C.