Acetic Anhydride → [4-(Trifluoromethyl)pyridin-2-yl]methyl acetate
反応式
[CH3:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[CH:4][N+:3]=1[O-].[C:13]([O:16]C(=O)C)(=[O:15])[CH3:14].C([O-])(O)=O.[Na+]>C(O)C>[C:13]([O:16][CH2:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[CH:4][N:3]=1)(=[O:15])[CH3:14]参加物
5
実験手順
2-Methyl-4-(trifluoromethyl)pyridine 1-oxide (4.0 g, 22 mmol) was added to acetic anhydride (12 mL) at 120° C. The mixture was refluxed for 1 h. To it was carefully added 10 mL of ethanol. Reflux was continued for 10 min. The mixture was poured into ice, neutralized with NaHCO3, and extracted with Et2O. The organic layer was dried (MgSO4) and concentrated. Chromatography on silica gel (5:2 hexanes/EtOAc) provided the product (3.4 g) as a brown oil. MS (M+H) 220.1.
後処理
- temperatureThe mixture was refluxed for 1 h
- temperatureReflux
- additionThe mixture was poured into ice
- extractionextracted with Et2O
- dry with materialThe organic layer was dried (MgSO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-f660664ddd1e4a429f1e2e674aa0422d
- 出典データセット
- uspto-grants-2014_04
- 特許番号
- US08697870B2
反応ノート
読み込み中…