反应详情

A mixture of intermediate (10) (0.00387 mole) and 1,1′-carbonylbis-1H-imidazole (0.0058 mole) in dichloromethane (40 ml) was stirred at RT for 90 minutes, then cyclohexylmethanol (0.0058 mole) was added. The mixture was stirred at RT overnight, diluted with CH2Cl2 and washed twice with an aqueous solution of NaCl. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/EtOAc 50/50). The pure fractions were collected and the solvent was evaporated. The residue was crystallized from EtOAc. The precipitate was filtered off, washed with DIPE and dried at 50° C. overnight, yielding 1.43 g of compound 7 with a molecular weight of 613.5, a melting point of 180° C. and represented by the formula wherein R14 is cyclohexylmethyl.

1. stirringThe mixture was stirred at RT overnight
2. washwashed twice with an aqueous solution of NaCl
3. customThe organic layer was separated
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customthe solvent was evaporated
7. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/EtOAc 50/50)
8. customThe pure fractions were collected
9. customthe solvent was evaporated
10. customThe residue was crystallized from EtOAc
11. filtrationThe precipitate was filtered off
12. washwashed with DIPE
13. customdried at 50° C. overnight