تفاعل #640574

معادلة التفاعل

water

3-(2-Nitrobenzylamino)-1-phenylpropanol

triethylamine

triphosgene

→

3-(2-nitrobenzyl)-6-phenyl-[1,3]-oxazinan-2-one

المردود 129.9%

المذيبات

toluene

toluene

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas slowly added dropwise
2. 2
   درجة الحرارةheated
3. 3
   درجة الحرارةto reflux for six hours
4. 4
   درجة الحرارةto cool
5. 5
   استخلاصextracted with ethyl acetate
6. 6
   غسيلThe organic layer was washed with 0.1N hydrochloric acid water
7. 7
   تجفيفdried over anhydrous sodium sulfate
8. 8
   أخرىthe solvent was evaporated under reduced pressure
9. 9
   غسيلThe residue was washed with a mixture of ether-ethyl acetate (1:2)

الإجراء التجريبي

3-(2-Nitrobenzylamino)-1-phenylpropanol (3.00 g, 10.5 mmol), triethylamine (4.24 g, 42.0 mmol) were dissolved in toluene (50 ml). Under ice cooled condition, a solution in which triphosgene (1.24 g, 4.19 mmol) was dissolved in toluene (5 ml) was slowly added dropwise thereto and heated to reflux for six hours after stirred at room temperature for one hour. The reaction mixture was poured into water and, after standing to cool, extracted with ethyl acetate. The organic layer was washed with 0.1N hydrochloric acid water and then dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The residue was washed with a mixture of ether-ethyl acetate (1:2) to obtain 3-(2-nitrobenzyl)-6-phenyl-[1,3]-oxazinan-2-one (1.70 g).

المصدر