反应 #640583

反应方程式

hydrochloric acid water

3-Aminopropanol

triethylamine

2-nitrobenzyl chloride

→

3-(2-nitrobenzylamino)propanol

收率 33.2%

溶剂

tetrahydrofuran

反应条件

后处理

1. 1
   温度After heated
2. 2
   温度to reflux for seven hours
3. 3
   温度to cool
4. 4
   萃取extracted with ether
5. 5
   萃取extracted with ethyl acetate
6. 6
   洗涤The organic layer was washed with a saturated brine
7. 7
   干燥dried over anhydrous sodium sulfate
8. 8
   其他the solvent was evaporated under reduced pressure

实验过程

3-Aminopropanol (3.94 g, 52.5 mmol) and triethylamine (1.77 g, 17.5 mmol) were dissolved in tetrahydrofuran (30 ml) and added with 2-nitrobenzyl chloride (3.00 g, 17.5 mmol) at room temperature. After heated to reflux for seven hours, the reaction mixture was allowed to cool and poured into 1N hydrochloric acid water and extracted with ether. The aqueous layer was adjusted to pH 9 with a saturated sodium hydrogen carbonate aqueous solution and then extracted with ethyl acetate. The organic layer was washed with a saturated brine and then dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to obtain 3-(2-nitrobenzylamino)propanol (1.22 g).

来源