反応 #640571

反応方程式

water

triethylamine

triphosgene

3-(2-Nitrobenzylamino)-1-propanol

→

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

収率 63.0%

溶媒

chloroform

反応条件

後処理

1. 1
   抽出extracted with ethyl acetate
2. 2
   洗浄after the organic layer was washed with a saturated brine, it
3. 3
   乾燥was dried over anhydrous sodium sulfate
4. 4
   その他the solvent was evaporated under reduced pressure
5. 5
   その他The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:4)

実験手順

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.

出典