反应 #1951070

反应方程式

(4-Fluorophenyl) divinyl phosphine oxide

benzylamine

→

1-benzyl-4-(4-fluorophenyl)-[1,4]azaphosphinane 4-oxide

收率 82.0%

溶剂

THF

water

反应条件

后处理

1. 1
   浓缩The reaction mixture was concentrated by rotary evaporation
2. 2
   萃取the product was extracted into dichloromethane
3. 3
   洗涤washed with saturated brine
4. 4
   干燥The organic phase was dried with sodium sulfate
5. 5
   过滤filtered
6. 6
   浓缩concentrated by rotary evaporation
7. 7
   其他to yield 2.52 g of crude product
8. 8
   其他Impurities were removed
9. 9
   洗涤The product was then eluted from the silica with 10% methanol in ethyl acetate
10. 10
    其他The solvents were removed by rotary evaporation

实验过程

(4-Fluorophenyl) divinyl phosphine oxide (1.50 g, 7.65 mmol) and benzylamine (1.05 mL, 9.57 mmol) were dissolved in a mixture of 100 mL of THF and 100 mL of deionized water. The reaction mixture was heated at 90° C. overnight. The reaction mixture was concentrated by rotary evaporation and the product was extracted into dichloromethane and washed with saturated brine. The organic phase was dried with sodium sulfate, filtered, and concentrated by rotary evaporation to yield 2.52 g of crude product. Impurities were removed by passing a solution of the crude product in ethyl acetate through a plug of silica. The product was then eluted from the silica with 10% methanol in ethyl acetate. The solvents were removed by rotary evaporation to yield 1.89 g (6.24 mmol, 82%) of 1-benzyl-4-(4-fluorophenyl)-[1,4]azaphosphinane 4-oxide as a colorless oil. ESMS (m/z): (M+1)+ found, 304.

来源