2,4,6-Trichloropyrimidine → 2,6-Dichloro-N-(5-methoxy-1H-pyrazol-3-yl)pyrimidin-4-amine
反応式
[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[C:4](Cl)[N:3]=1.Cl.[CH3:11][O:12][C:13]1[NH:17][N:16]=[C:15]([NH2:18])[CH:14]=1>C(O)C>[Cl:1][C:2]1[N:3]=[C:4]([NH:18][C:15]2[CH:14]=[C:13]([O:12][CH3:11])[NH:17][N:16]=2)[CH:5]=[C:6]([Cl:8])[N:7]=1参加物
4
実験手順
To a solution of 2,4,6-trichloro-pyrimidine (1.7 g) in absolute ethanol (100 mL) was added DIEPA (4.1 mL) and 5-methoxy-1H-pyrazol-3-amine hydrogen chloride salt (1.46 g). The resulting solution was stirred at room temperature for over night. The solvent was evaporated under reduced pressure. The crude compound was purified by Gilson (10-60% MeCN/H2O, 15 minutes) to give the titled compound as solid (1.23 g). 1H NMR δ 12.19 (s, 1H) 10.68 (s, 1H) 6.76 (s, 1H) 5.40 (s, 1H) 3.82 (s, 3H); m/z 260.
後処理
- customThe solvent was evaporated under reduced pressure
- customThe crude compound was purified by Gilson (10-60% MeCN/H2O, 15 minutes)
出典と根拠
- ORDレコード
- ord-dbc94f7fa6114182a36cb1499267bc72
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08088784B2
反応ノート
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