Dichloromethane → 4,6-Dichloro-2-methylpyrimidine
反応式
O[C:2]1[CH:7]=C(O)[N:5]=[C:4]([CH3:9])[N:3]=1.P(Cl)(Cl)([Cl:12])=O.Cl[CH2:16][Cl:17]>>[Cl:12][C:2]1[CH:7]=[C:16]([Cl:17])[N:5]=[C:4]([CH3:9])[N:3]=1参加物
4
反応条件
- 温度
- 95 °C
実験手順
4,6-Dihydroxy-2-methylpyrimidine 21 (1.03 g, 8.1 mmol) is suspended in 2.5 mL phosphorus oxychloride (27.3 mmol). The mixture is heated to 95° C. for 18 hours. Upon cooling, the mixture is diluted with dichloromethane (100 mL) and filtered. It is then washed with water, saturated aqueous sodium bicarbonate and brine, then concentrated to yield 4,6-dichloro-2-methylpyrimidine 22 as a white powder. 1H-NMR (400 MHz, CDCl3) δ=7.45 (s, 1H), 2.77 (s, 3H). MS calculated for C5H5Cl2N2 (M+H+) 162.99. found 163.2.
後処理
- temperatureUpon cooling
- filtrationfiltered
- washIt is then washed with water, saturated aqueous sodium bicarbonate and brine
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-9f9d73ccab04499d925e69c5dfa51904
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07745445B2
反応ノート
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