Water → 4,5-Diamino-2,6-dichloropyrimidine
反応式
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[C:6]([Cl:11])[N:5]=[C:4]([Cl:12])[N:3]=1.[H][H].O>CO.[Ni]>[NH2:1][C:2]1[C:7]([NH2:8])=[C:6]([Cl:11])[N:5]=[C:4]([Cl:12])[N:3]=1参加物
6
実験手順
To a solution of 4-amino-2,6-dichloro-5-nitropyrimidine, prepared as described in a), in methanol (30 ml), was added Raney nickel freshly prepared from 500 mg of alloy. The reaction mixture was stirred 20 hours in the hydrogen atmosphere. Then a new catalyst, prepared from 500 mg of alloy, was added and the reaction mixture was stirred next 24 hours in the hydrogen atmosphere. The catalyst was removed, the reaction mixture was concentrated in vacuo and the residue was extracted with hot water. Product, which was obtained after cooling of the water solution, was purified by chromatography (SiO2, VI—1:1)
後処理
- customfreshly prepared from 500 mg of alloy
- customThen a new catalyst, prepared from 500 mg of alloy
- additionwas added
- customThe catalyst was removed
- concentrationthe reaction mixture was concentrated in vacuo
- extractionthe residue was extracted with hot water
- customProduct, which was obtained
- customwas purified by chromatography (SiO2, VI—1:1)
出典と根拠
- ORDレコード
- ord-bbf78615fbb84d04a4247fe9d4e89db0
- 出典データセット
- uspto-grants-2010_10
- 特許番号
- US07816350B2
反応ノート
読み込み中…