反応式
[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.S(S([O-])=O)([O-])=O.[Na+].[Na+]>O>[NH2:12][C:3]1[C:4](=[O:11])[N:5]([CH3:10])[C:6](=[O:9])[N:7]([CH3:8])[C:2]=1[NH2:1]参加物
4
反応条件
- 温度
- 80 °C
実験手順
Crude 6-amino-1,3-dimethyl-5-nitroso-1H-pyrimidine-2,4-dione (5 mmol) was suspended in water (7 mL) at 40° C. and treated with sodium dithionite (17.5 mmol). After 20 minutes at 40° C. the reaction mixture was warmed to 80° C. for 30 mins and then cooled in ice for 30 mins. The precipitate was isolated by filtration, washed with cold water and dried in vacuo to give crude 5,6-diamino-1,3-dimethyl-1H-pyrimidine-2,4-dione as a light beige solid which was of sufficient purity for subsequent use without additional purification (80%).
後処理
- temperaturecooled in ice for 30 mins
- customThe precipitate was isolated by filtration
- washwashed with cold water
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-258c8d66a8f241d58aabee1e94821152
- 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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