反应 #640580

反应方程式

water

triethylamine

thiophosgene

2,2-Dimethyl-3-(2-nitrobenzylamino)-1-propanol

→

5,5-dimethyl-3-(2-nitrobenzyl)-[1,3]-oxazinan-2-thione

收率 88.8%

溶剂

chloroform

反应条件

后处理

1. 1
   workup.STIRRINGstirred at room temperature for one hour
2. 2
   萃取extracted with ethyl acetate
3. 3
   洗涤The organic layer was washed with a saturated brine
4. 4
   干燥dried over anhydrous sodium sulfate
5. 5
   其他the solvent was evaporated under reduced pressure
6. 6
   其他The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1)

实验过程

2,2-Dimethyl-3-(2-nitrobenzylamino)-1-propanol (1.07 g, 4.50 mmol) was dissolved in chloroform (20 ml) and the reaction solution was cooled to 0° C. Then triethylamine (1.82 g, 18.0 mmol), thiophosgene (0.52 g, 4.50 mmol) was added thereto and stirred at a temperature as is for two hours and at room temperature for one hour. The reaction mixture was added with water, stirred at room temperature for one hour 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. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1) to obtain 5,5-dimethyl-3-(2-nitrobenzyl)-[1,3]-oxazinan-2-thione (1.12 g).

来源