반응 #640571

반응 방정식

water

triethylamine

triphosgene

3-(2-Nitrobenzylamino)-1-propanol

→

3-(2-nitrobenzyl)-[1,3]-oxazinan-2-one

수율 63.0%

용매

chloroform

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate
2. 2
   세척after the organic layer was washed with a saturated brine, it
3. 3
   건조was dried over anhydrous sodium sulfate
4. 4
   기타the solvent was evaporated under reduced pressure
5. 5
   기타The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:4)

실험 절차

3-(2-Nitrobenzylamino)-1-propanol (1.03 g, 4.90 mmol) was dissolved in chloroform (20 ml) and the reaction solution was cooled to 0° C. Then triethylamine (1.98 g, 19.6 mmol), triphosgene (0.58 g, 1.95 mmol) were added thereto and the mixture was stirred at the same temperature for 1.5 hours. The reaction mixture was added with water and extracted with ethyl acetate and after the organic layer was washed with a saturated brine, it was 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=1:4) and 3-(2-nitrobenzyl)-[1,3]-oxazinan-2-one (0.29 g) was obtained.

출처