Acetic Anhydride → 1-(4-Chloro-2-methylphenyl)-3-methyl-1,3-diazinane-2,4-dione
반응식
[CH3:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]([N:12]([CH3:18])[CH2:13][CH2:14][C:15](O)=O)=[O:11].C(OC(=O)C)(=[O:21])C>>[CH3:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[N:9]1[CH2:15][CH2:14][C:13](=[O:21])[N:12]([CH3:18])[C:10]1=[O:11]참가 물질
3
실험 절차
At first, 8.0 g (0.03 moles) of N-(2-methyl-4-chlorophenylcarbamoyl)-N-methyl-β-alanine was added to 250 ml of acetic anhydride, and the mixture was refluxed with heating for 2.5 hours. Acetic anhydride was removed therefrom by distillation under reduced pressure, and precipitated crystals were recrystallized from 60 ml of ethyl acetate and 150 ml of n-hexane, whereby 1.8 g of the desired compound was obtained as crystals having a melting point of 120° to 127° C. (yield: 24.1%).
후처리
- temperaturethe mixture was refluxed
- temperaturewith heating for 2.5 hours
- customAcetic anhydride was removed
- distillationby distillation under reduced pressure