Phosgene → N-(4,6-dimethylpyrimidin-2-yl)-N-phenylcarbamoyl chloride
反応式
Cl.[NH:2]([C:9]1[N:14]=[C:13]([CH3:15])[CH:12]=[C:11]([CH3:16])[N:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:17](Cl)([Cl:19])=[O:18]>C1(C)C=CC=CC=1>[CH3:15][C:13]1[CH:12]=[C:11]([CH3:16])[N:10]=[C:9]([N:2]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:17]([Cl:19])=[O:18])[N:14]=1参加物
4
実験手順
2-Anilino-4,6-dimethylpyrimidine hydrochloride (100 g) was suspended in toluene (1200 ml). A slow stream of phosgene was passed through this over 5.5 hours at 108° (bath temperature of 120°) and then stirred for a further hour at the same temperature. After standing overnight, c. 300 ml of toluene was distilled at a bath temperature of 150°. It was then evaporated under reduced pressure. The oily residue was extracted twice with hexane (1000 ml) and the solution concentrated under reduced pressure. After a period of time crystals formed and these were separated to give N-(4,6-dimethylpyrimidin-2-yl)-N-phenylcarbamoyl chloride. This was shown by thin layer chromatography to be a uniform product, which was used without further purification.