反应详情

5 g (11 mmol) of tert.butyl (S)-11,12,13,13a-tetrahydro-8-iodo-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate, 30 g (300 mmol) of cyclohexanol and 1 g (4 mmol) of tetraethyl orthotitanate are stirred at 125° overnight, the solution is evaporated to dryness and the residue is taken up in chloroform. The solution is then stirred for 0.5 hour with 40 ml of a saturated potassium fluoride solution, the resulting emulsion is filtered over siliceous earth, the organic phase is separated, washed with water, dried over magnesium sulphate and evaporated. By crystallization from ethyl acetate there is obtained cyclohexyl (S)-11,12,13,13a-tetrahydro-8-iodo-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate of melting point 181°-182°.

1. customthe solution is evaporated to dryness
2. filtrationthe resulting emulsion is filtered over siliceous earth
3. customthe organic phase is separated
4. washwashed with water
5. dry with materialdried over magnesium sulphate
6. customevaporated
7. customBy crystallization from ethyl acetate