反应详情

A mixture of 0.31 g. of 55% sodium hydride-mineral oil dispersion and 0.65 g. of N-(2-chloroethyl)morpholine hydrochloride in 25 ml. of dry dimethylformamide is stirred at room temperature for 0.5 hours. To the mixture is added 0.40 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 dryness and the solid residue is recrystallized from ethyl acetate-hexane to give white crystals, m.p. 109°-111°C.

1. additionA mixture of 0.31 g
2. additionTo the mixture is added 0.40 g
3. temperatureThe reaction mixture is cooled
4. customquenched with water
5. extractionextracted with chloroform
6. concentrationThe dried chloroform extracts are concentrated to dryness
7. customthe solid residue is recrystallized from ethyl acetate-hexane
8. customto give white crystals, m.p. 109°-111°C.