反应详情

A mixture of 0.47 g. of 55% sodium hydride-mineral oil dispersion and 0.83 g. of 2-dimethylamino-1-methylethylchloride hydrochloride in 30 ml. of dry dimethylformamide is stirred at room temperature for 0.5 hours. To the mixture is added 0.6 g. of 4,9-dihydro-4-methyl-10H-thieno[3,4-b][1,5]-benzodiazepin-10-one and stirring is continued for 18 hours. The reaction mixture is cooled, quenched with water and extracted with chloroform. The dried chloroform extracts are concentrated to an oil which is chromatographed on silica gel preparative thin layer chromatographic (tlc) plates using 10:1 benzene:methanol to give a yellow oil. The oil is dissolved in ethanol and treated with anhydrous hydrogen chloride followed by dilution with ether to give a solid, which is recrystallized from ethanol to give white crystals, m.p. 280°-282° C. (dec.).

1. additionA mixture of 0.47 g
2. additionTo the mixture is added 0.6 g
3. temperatureThe reaction mixture is cooled
4. customquenched with water
5. extractionextracted with chloroform
6. concentrationThe dried chloroform extracts are concentrated to an oil which
7. customis chromatographed on silica gel preparative thin layer chromatographic (tlc) plates
8. custommethanol to give a yellow oil
9. customto give a solid, which
10. customis recrystallized from ethanol
11. customto give white crystals, m.p. 280°-282° C. (dec.)