反应详情

A mixture of 0.3 g. of 55% sodium hydride-mineral oil dispersion and 0.35 g. of 4,9-dihydro-4-methyl-10H-thieno-[3,4-b][1,5]benzodiazepin-10-one in 25 ml. of dry dimethylformamide is stirred at room temperature for 0.5 hours. To the mixture is added 0.45 g. of dimethylaminopropyl chloride and stirring at room temperature is continued for 18 hours. The reaction mixture is cooled, quenched with water, acidified, decolorized and filtered. The filtrate is made alkaline and extracted with chloroform. The dried chloroform extracts are concentrated under reduced pressure to give an oil which is crystallized by dissolving in boiling hexane and a minimal volume of ethyl acetate and cooling to give off-white crystals, m.p. 52°-56° C.

1. additionA mixture of 0.3 g
2. additionTo the mixture is added 0.45 g
3. temperatureThe reaction mixture is cooled
4. customquenched with water
5. filtrationfiltered
6. extractionextracted with chloroform
7. concentrationThe dried chloroform extracts are concentrated under reduced pressure
8. customto give an oil which
9. customis crystallized
10. dissolutionby dissolving
11. temperaturea minimal volume of ethyl acetate and cooling
12. customto give off-white crystals, m.p. 52°-56° C.