反应详情

41.20 g (112.1 mmol) of 1-[[(S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-1-yl]carbonyl]imidazole and 12.6 g (123.4 mmol) of butyramidoxime are stirred at 60° for 2.5 hours in 200 ml of N,N-dimethylformamide. The cooled suspension is then filtered; the filter residue is rinsed with ether and dried. The product obtained is stirred at 1120° for 3 hours with 350 ml of glacial acetic acid. The reaction mixture is evaporated and the residue is dissolved in methylene chloride. The solution is washed with a saturated sodium bicarbonate solution, dried over magnesium sulphate and evaporated. By recrystallization of the residue from methylene chloride and ethyl acetate there is obtained (S)-8-chloro-11,12,13,13a-tetrahydro-1-(3-propyl-1,2,4-oxadiazol-5-yl)-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]-benzodiazepin-9-one of melting point 176°-178°.

1. filtrationThe cooled suspension is then filtered
2. washthe filter residue is rinsed with ether
3. customdried
4. customThe product obtained
5. customThe reaction mixture is evaporated
6. dissolutionthe residue is dissolved in methylene chloride
7. washThe solution is washed with a saturated sodium bicarbonate solution
8. dry with materialdried over magnesium sulphate
9. customevaporated
10. customBy recrystallization of the residue from methylene chloride and ethyl acetate