反应详情

A stirred solution of potassium hydroxide (3.37 g., 0.06 mole) in methanol (30 ml.) is cooled in an ice bath, under nitrogen, and treated with (cyclopropylmethyl)-amine hydrochloride (6.45 g., 0.06 mole). The resulting mixture is kept in the ice bath for 15 minutes, treated with tetrahydrofuran (250 ml.), 8-(trifluoromethyl)-1-(chloromethyl)-6-(o-chlorophenyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine (6.86 g., 0.02 mole) and potassium iodide (3.32 g., 0.02 mole) and kept at ambient temperature for 18 hours. The mixture is concentrated and the residue is mixed with water and extracted with methylene chloride. The extract is washed with brine, dried over anhydrous sodium sulfate and concentrated. The product is crystallized once from ethyl acetate and once from methylene chloride ethyl acetate to give 8-(trifluoromethyl)-1-[[(cyclopropylmethyl)amino]methyl]-6-(o-chlorophenyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine. Preparation 28 8 -Chloro-1-[[(cyclopropylmethyl)amino] methyl]-6-(o-chlorophenyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine

1. concentrationThe mixture is concentrated
2. additionthe residue is mixed with water
3. extractionextracted with methylene chloride
4. washThe extract is washed with brine
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customThe product is crystallized once from ethyl acetate and once from methylene chloride ethyl acetate