反応式
[NH2:1][C:2]1[N:7]([CH3:8])[C:6](=[O:9])[N:5]([CH3:10])[C:4](=[O:11])[CH:3]=1.[N:12]([O-])=[O:13].[Na+]>O>[NH2:1][C:2]1[N:7]([CH3:8])[C:6](=[O:9])[N:5]([CH3:10])[C:4](=[O:11])[C:3]=1[N:12]=[O:13]参加物
4
反応条件
- 温度
- 80 °C
実験手順
Commercially available 6-amino-1,3-dimethyl-1H-pyrimidine-2,4-dione (10 mmol) was dissolved in 1:1 water/glacial acetic acid (50 mL total volume) at 80° C. and sodium nitrite (20 mmol) added in portions. After the addition was complete the reaction mixture was stirred at 80° C. for 1 hr. Cooled in ice for 30 mins then filtered and washed with water. The precipitate was dried in vacuo to give crude 6-amino-1,3-dimethyl-5-nitroso-1H-pyrimidine-2,4-dione as a red-violet colored solid which was of sufficient purity for subsequent use without additional purification (89%).
後処理
- additionAfter the addition
- temperatureCooled in ice for 30 mins
- filtrationthen filtered
- washwashed with water
- customThe precipitate was dried in vacuo
出典と根拠
- ORDレコード
- ord-f528c07c773b459ea5585eff18503e09
- 出典データセット
- uspto-grants-2006_12
- 特許番号
- US07148229B2
関連ノート
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