反应详情

3.5 g (7.7 mmol) of tert.butyl (S)-12,12a-dihydro-8-iodo-9-oxo-9H,11H-azeto[2,1-c]imidazo[1,5-a][1,4]benzodiazepine-1-carboxylate, 10 g (116 mmol) of cyclopentanol and 0.8 g (3 mmol) of tetraethyl orthotitanate are stirred at 125° overnight, the solution obtained is evaporated and the residue is taken up in chloroform. The solution obtained is 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 a rapid filtration through about 200 g of silica gel while eluting with ethyl acetate and subsequent crystallization from ethyl acetate there is obtained cyclopentyl (S)-12,12a-dihydro-8-iodo-9-oxo-9H,11H-azeto[2,1-c]imidazo[1,5-a][1,4]benzodiazepine-1-carboxylate of melting point 184°-185°.

1. customthe solution obtained
2. customis evaporated
3. customThe solution obtained
4. filtrationthe resulting emulsion is filtered over siliceous earth
5. customthe organic phase is separated
6. washwashed with water
7. dry with materialdried over magnesium sulphate
8. customevaporated
9. filtrationBy a rapid filtration through about 200 g of silica gel
10. washwhile eluting with ethyl acetate and subsequent crystallization from ethyl acetate