Acetic Anhydride → [4-(Trifluoromethyl)pyridin-2-yl]methyl acetate
반응식
[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]참가 물질
5
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-f660664ddd1e4a429f1e2e674aa0422d
- 출처 데이터셋
- uspto-grants-2014_04
- 특허 번호
- US08697870B2
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