Phosphorus oxychloride → HCID 70454969、化合物
反応式
[C:1]([NH:4][CH2:5][C:6]1[NH:7][C:8](=[O:13])[NH:9][C:10](=O)[CH:11]=1)(=O)[CH3:2].P(Cl)(Cl)([Cl:16])=O>>[Cl:16][C:10]1[CH:11]=[C:6]2[CH:5]=[N:4][CH:1]([CH3:2])[N:7]2[C:8](=[O:13])[N:9]=1参加物
3
実験手順
A suspension of 6.63 g (36.2 mmole) of 4-acetylaminomethylpyrimidine-2,6-dione in 250 ml of phosphorous oxychloride was heated at reflux for 20 hours, and was then cooled and evaporated. The residue was added to about 700 ml of cold saturated sodium bicarbonate solution. To the resulting mixture was added 200 ml of chloroform and sufficient solid sodium bicarbonate to neutralize the mixture. The solid was separated by filtration, and the filtrate was saved for Part B. The solid was washed with water and ethanol, and was then recrystallized from ethanol to provide yellow solid 7-chloro-3-methylimidazo[1,5-c]pyrimidin-5-one, m.p. 239° C. (dec.). Analysis: Calculated for C7H6ClN3O; %C, 45.8; %H, 3.3; %N, 22.9; Found; %C, 45.8; %H, 3.1; %N, 22.8.
後処理
- temperaturewas heated
- temperature