反应详情

A mixture of 2.22 g (8 mmol) of 7-chloro-4,5-dihydro-3-(hydroxymethyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one, 0.6 ml (10 mmoL) of methyl iodide and 20 ml of dry dimethylformamide is treated with 0.4 g (9 mmol) of sodium hydride (55 percent oil dispersion, washed with n-hexane) and the mixture is stirred at room temperature for 23 hours. The mixture is poured into 50 ml of water and extracted four times with methylene chloride. The methylene chloride solution is dried over magnesium sulphate and evaporated. The crude product is chromatographed on silica gel using methylene chloride containing 1% of methanol for the elution. By subsequent recrystallization from ethyl acetate/n-hexane there is obtained 7-chloro-4,5-dihydro-3-(methoxymethyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one of melting point 143°-144°.

1. extractionextracted four times with methylene chloride
2. dry with materialThe methylene chloride solution is dried over magnesium sulphate
3. customevaporated
4. customThe crude product is chromatographed on silica gel
5. washfor the elution
6. customBy subsequent recrystallization from ethyl acetate/n-hexane there