반응 #94098

반응 방정식

N,O-dimethylhydroxylamine

4-(4-isopropylphenethyloxy)phenylcarbamyl chloride

pyridine

→

N'-[4-(4-isopropylphenethyloxy)phenyl]-N-methoxy-N-methylurea

수율 42.0%

용매

toluene

toluene

반응 조건

후처리

1. 1
   기타at a temperature below 20° C
2. 2
   온도The mixture is heated
3. 3
   온도under reflux for 4 hours
4. 4
   세척the separated organic layer is washed with dilute hydrochloric acid
5. 5
   세척thoroughly washed with water
6. 6
   건조dried over anhydrous sodium sulfate
7. 7
   기타The solvent is removed under reduced pressure
8. 8
   기타the crude crystals are recrystallized from ethanol

실험 절차

Into a solution of 10.6 g of 4-(4-isopropylphenethyloxy)phenylcarbamyl chloride in 200 ml of toluene are added 4 ml of pyridine and a solution of 2.5 g of N,O-dimethylhydroxylamine in 50 ml of toluene at a temperature below 20° C. The mixture is heated under reflux for 4 hours. The reaction mixture is then poured into ice water, and the separated organic layer is washed with dilute hydrochloric acid, thoroughly washed with water and dried over anhydrous sodium sulfate. The solvent is removed under reduced pressure, and the crude crystals are recrystallized from ethanol to obtain 4.8 g of N'-[4-(4-isopropylphenethyloxy)phenyl]-N-methoxy-N-methylurea as white needles, M.P. 81°-82° C.

출처