反応式
[Cl:1][C:2]1[C:7]([CH3:8])=[C:6](Cl)[N:5]=[C:4]([CH3:10])[N:3]=1.[OH-].[NH4+:12]>C(O)C>[Cl:1][C:2]1[N:3]=[C:4]([CH3:10])[N:5]=[C:6]([NH2:12])[C:7]=1[CH3:8]参加物
4
反応条件
- 温度
- 80 °C
実験手順
A microwave vial was charged with 4,6-dichloro-2,5-dimethylpyrimidine (523 mg, 2.95 mmol) and ammonium hydroxide (8 mL) in ethanol (4 mL). The vial was heated to 80° C. and stirred for 8 h. After concentration under reduced pressure, the reaction mixture was extracted with EtOAc (15 mL×8). The combined organic layers were washed with brine (30 mL), dried over Na2SO4 and concentrated to give 6-chloro-2,5-dimethylpyrimidin-4-amine as a yellow solid (411 mg). MS (ESI): m/z 158 [M+H]+.
後処理
- concentrationAfter concentration under reduced pressure
- extractionthe reaction mixture was extracted with EtOAc (15 mL×8)
- washThe combined organic layers were washed with brine (30 mL)
- dry with materialdried over Na2SO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-ea626cb6c9be42e284ebcf6abfc8c613
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08969349B2
関連ノート
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