反应详情

温度

40 °C

9a-(1H-Imidazol-4-yl)-1,2,3,4,4a,9a-hexahydrofluoren-9-one (0.41 g) was dissolved in ethanol (10 ml). 48% NaOH solution (0.003 ml) and NaBH4 (0.06 g) was added and the mixture was heated at 40° C. for 12 hours. Water (2.5 ml) was added and the mixture was cooled to the ambient temperature. HCl (0.3 ml of 30% HCl in 1 ml H2O) was added and the mixture was stirred for 5 minutes. NaOH (0.2 ml of 48% NaOH in 5 ml H2O) was then added and the solvents were evaporated. The residue was mixed with water (30 ml) and extracted with CH2Cl2 (3×30 ml) and evaporated. The crude product was purified by flash chromatography using methylene chloride/methanol (95:5) as eluent. The yield was 0.26 g.

1. temperaturethe mixture was cooled to the ambient temperature
2. customthe solvents were evaporated
3. additionThe residue was mixed with water (30 ml)
4. extractionextracted with CH2Cl2 (3×30 ml)
5. customevaporated
6. customThe crude product was purified by flash chromatography