反应详情

温度

23 °C

A mixture containing 1-(4-(3-bromophenyl)-1H-imidazol-2-yl)-5-methyl-1-hexanamine (obtained at stage 13777.3; 0.8 g; 0.0019 mol), triethylamine (0.4 ml; 0.003 mol) and cyclohexanone (0.32 ml; 0.0023 mol) in 10 ml methanol was agitated for about 30 minutes at about 23° C. Sodium triacetoxyborohydride (630 mg; 0.003 mol) was then added. The reaction mixture was agitated for about 16 hours and then poured into water. After extraction with ethyl acetate, the organic phase was washed with a saturated sodium chloride solution and then dried over magnesium sulfate. The solvent was evaporated and the residue purified over a silica column (eluent: mixture CH2Cl2—MeOH/95-05). A white-colored powder was obtained with a yield of 38%. Melting point: 236-238° C. MH+=418.2.

1. stirringThe reaction mixture was agitated for about 16 hours
2. extractionAfter extraction with ethyl acetate
3. washthe organic phase was washed with a saturated sodium chloride solution
4. dry with materialdried over magnesium sulfate
5. customThe solvent was evaporated
6. customthe residue purified over a silica column (eluent: mixture CH2Cl2—MeOH/95-05)
7. customA white-colored powder was obtained with a yield of 38%