反应详情

温度

60 °C

Sodium borohydride (0.15 g) is added to a suspension of 1-benzyl-4-methyl-9H-indeno[2,1-b]pyridinium bromide (0.92 g) in ethanol (10 mL) chilled in an ice bath. The cooling bath is removed and the mixture is stirred at room temperature for 1 h and at 60° C. for 2 h. More sodium borohydride (0.18 g) is added and stirring is continued at reflux temperature for 4 h. After the addition of another portion of sodium borohydride (0.10 g), the mixture is stirred at reflux temperature overnight. After cooling to room temperature, ice-cold water is added and the precipitate is separated by filtration. The precipitate is dissolved in ether, the resulting solution is dried (Na2SO4), and the solvent is evaporated to afford the crude product that is used without further purification. Yield: 0.66 g (crude); Mass spectrum (ESI+): m/z=276 [M+H]+.

1. temperaturechilled in an ice bath
2. customThe cooling bath is removed
3. additionMore sodium borohydride (0.18 g) is added
4. stirringstirring
5. temperatureat reflux temperature for 4 h
6. additionAfter the addition of another portion of sodium borohydride (0.10 g)
7. stirringthe mixture is stirred
8. temperatureat reflux temperature overnight
9. temperatureAfter cooling to room temperature
10. additionice-cold water is added
11. customthe precipitate is separated by filtration
12. dissolutionThe precipitate is dissolved in ether
13. dry with materialthe resulting solution is dried (Na2SO4)
14. customthe solvent is evaporated