4,6-Dichloropyrimidine → 4-Chloro-6-(methylsulfanyl)pyrimidine
反応式
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]=[CH:4][N:3]=1.[CH3:9][S-:10].[Na+]>C1COCC1.C(OCC)(=O)C.O>[Cl:1][C:2]1[CH:7]=[C:6]([S:10][CH3:9])[N:5]=[CH:4][N:3]=1参加物
6
反応条件
- 温度
- 60 °C
実験手順
To a solution of 4,6-dichloro-pyrimidine (10.0 g, 67 mmol) in THF (55 ml), sodium thiomethylate (5.175 g, 74 mmol) is added under inert gas atmosphere. The reaction mixture is stirred at 60° C. overnight. After cooling down to r.t., the reaction mixture is diluted with ethyl acetate and water (100 ml each). The organic phase is removed and the aqueous phase is extracted with ethyl actetate. The combined organic phases are washed and dried, and the solvent is evaporated to give 9.74 g (90%) of a pale yellow solid (contains ca. 9% of starting material and ca. 9% of 4,6-dimethylsulfanyl-pyrimidine) which is used without any further purification.
後処理
- temperatureAfter cooling down to r.t.
- customThe organic phase is removed
- extractionthe aqueous phase is extracted with ethyl actetate
- washThe combined organic phases are washed
- customdried
- customthe solvent is evaporated
出典と根拠
- ORDレコード
- ord-e94874e78eb84824a8768f65a083e4fc
- 出典データセット
- uspto-grants-2011_12
- 特許番号
- US08080552B2
反応ノート
読み込み中…