Methanol → 4-Chloro-2-methoxy-6-methylpyrimidine
反応式
[Na].Cl[C:3]1[N:8]=[C:7]([Cl:9])[CH:6]=[C:5]([CH3:10])[N:4]=1.[OH2:11].[CH3:12]O>>[Cl:9][C:7]1[CH:6]=[C:5]([CH3:10])[N:4]=[C:3]([O:11][CH3:12])[N:8]=1参加物
5
実験手順
To anhydrous methanol (10 ml) was added sodium (230 mg, 10 mmol) and the mixture was stirred under an argon atmosphere until a clear solution had formed. This solution was added dropwise over two hours with stirring to a solution of 2,4-dichloro-6-methylpyrimidine (1.79 g, 11 mmol) in anhydrous methanol (10 ml) under cooling so that the temperature remained below 10° C. Stirring was continued for 30 minutes, then water was added (2 ml), the mixture was filtered and the filtrate was evaporated to dryness under reduced pressure. The residue was purified by column chromatography (pre-packed silica column, gradient of heptane/ethyl acetate). 750 mg was obtained (4.75 mmol, 47%). MS (APCI) m/z=159.2 [M+H]+.
後処理
- customhad formed
- additionThis solution was added dropwise over two hours
- temperatureunder cooling so that the temperature
- customremained below 10° C
- stirringStirring
- filtrationthe mixture was filtered
- customthe filtrate was evaporated to dryness under reduced pressure
- customThe residue was purified by column chromatography (pre-packed silica column, gradient of heptane/ethyl acetate)
- custom750 mg was obtained (4.75 mmol, 47%)
出典と根拠
- ORDレコード
- ord-ff1bbdd973f8423086e675f8be01fd11
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08877934B2
反応ノート
読み込み中…