反应 #1914852

反应方程式

4-cyano-2,6-difluorobenzyl methanesulfonate

4-Cyano-2,6-difluorobenzyl methanesulfonate

sodium azide

DMF

→

4-Azidomethyl-2,6-difluorobenzonitrile

溶剂

water

water

反应条件

后处理

1. 1
   萃取extracted three times with diethyl ether
2. 2
   洗涤The combined ethereal phase was washed five times with water
3. 3
   干燥dried (Na2SO4)
4. 4
   其他evaporated
5. 5
   其他A small sample was evaporated for NMR purposes
6. 6
   其他the product crystallised
7. 7
   其他The rest was evaporated cautiously but not until complete dryness
8. 8
   其他Yield (theoretically 1.26 g)

实验过程

A mixture of 4-cyano-2,6-difluorobenzyl methanesulfonate (1.61 g, 6.51 mmol; see step (xii) above) and sodium azide (0.72 g, 0.0111 mol) in 10 mL of water and 20 mL of DMF was stirred at room temperature overnight. The resultant was subsequently poured into 200 mL of water and extracted three times with diethyl ether. The combined ethereal phase was washed five times with water, dried (Na2SO4) and evaporated. A small sample was evaporated for NMR purposes and the product crystallised. The rest was evaporated cautiously but not until complete dryness. Yield (theoretically 1.26 g) was assumed to be almost quantitative based on NMR and analytical HPLC.

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