反应详情

温度

80 °C

To a solution of 3-bromobenzonitrile (0.91 g, 5 mmol) in dioxane (19 mL), NaBO3.4H2O (2.12 g, 13.78 mmol) and H2O (19 mL) were added. The mixture was stirred at 80° C. 16 hours (h), cooled, added of H2O and extracted with CH2Cl2. The combined organic layers were dried over Na2SO4 and evaporated. Purification of the residue by column chromatography (hexane/EtOAc 2:8) and recrystallization gave the desired product as colorless tablets. Yield 80% (EtOH). Mp: 156–7° C. (lit. 156° C.) (Pearson, D. E. et al., J. Org. Chem., 28: 3147–3149, (1963)). MS (EI): m/z 199 (M+); 183 (100%).

1. temperature16 hours (h), cooled
2. extractionextracted with CH2Cl2
3. dry with materialThe combined organic layers were dried over Na2SO4
4. customevaporated
5. customPurification of the residue
6. customby column chromatography (hexane/EtOAc 2:8) and recrystallization