Sodium chlorodifluoroacetate → 2-Chloro-5-(difluoromethoxy)pyrimidine
反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([OH:8])=[CH:4][N:3]=1.Cl[C:10]([F:15])([F:14])C([O-])=O.[Na+]>CN(C)C=O.O>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([O:8][CH:10]([F:15])[F:14])=[CH:4][N:3]=1参加物
5
実験手順
2-Chloropyrimidin-5-ol (1 g, 7.66 mmol) and sodium 2-chloro-2,2-difluoroacetate (3.50 g, 22.98 mmol) in N,N-dimethylformamide (20 mL) and water (0.2 mL) were heated to 90° C. for 24 hours and concentrated in vacuo. The residue was purified by column chromatography (5-30% ethyl acetate/hexanes) to afford 2-chloro-5-(difluoromethoxy)pyrimidine (549 mg, 3.04 mmol, 39.7% yield) as a pale yellow oil. MS (LC/MS) R.T.=1.32; [M+H]+=181.14.
後処理
- concentrationconcentrated in vacuo
- customThe residue was purified by column chromatography (5-30% ethyl acetate/hexanes)
出典と根拠
- ORDレコード
- ord-2a819fa1099a495e931c10e7130674e9
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08309577B2
反応ノート
読み込み中…