Water → 6-Amino-5-nitroso-1-pentyl-2-thioxo-2,3-dihydropyrimidin-4(1H)-one
反応式
[NH2:1][C:2]1[N:7]([CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[C:6](=[S:13])[NH:5][C:4](=[O:14])[CH:3]=1.[N:15]([O-])=[O:16].[Na+].O>C(O)(=O)C>[NH2:1][C:2]1[N:7]([CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[C:6](=[S:13])[NH:5][C:4](=[O:14])[C:3]=1[N:15]=[O:16]参加物
5
反応条件
- 温度
- 75 °C
実験手順
6-Amino-1-pentyl-2-thioxo-2,3-dihydropyrimidin-4(1H)-one (8.0 g, 0.038 mol) was mixed with sodium nitrite (3.1 g, 0.045 mol) in acetic acid (120 mL). The mixture was stirred at 75° C. for 1 h. The color of the reaction mixture became pink and then purple. The solution was allowed to cool down to room temperature, and water (40 mL) was added. The solid was collected by suction filtration and washed with water (50 mL) to produce the desired product, which was used directly for next step without further purification. LCMS calculated for C9H15N4O2S: (M+H) 243.1; found 243.1.
後処理
- temperatureto cool down to room temperature
- filtrationThe solid was collected by suction filtration
- washwashed with water (50 mL)
出典と根拠
- ORDレコード
- ord-866cc9a3907a4cf9b04e7b8ada8932cc
- 出典データセット
- uspto-grants-2009_03
- 特許番号
- US07511050B2
反応ノート
読み込み中…