تفاعل #640571

معادلة التفاعل

water

triethylamine

triphosgene

3-(2-Nitrobenzylamino)-1-propanol

→

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

المردود 63.0%

المذيبات

chloroform

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر