4-Hydroxybenzaldehyde → 4-(2,2-Difluoroethoxy)benzaldehyde
반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.FC(F)(F)S(O[CH2:16][CH:17]([F:19])[F:18])(=O)=O.C([O-])([O-])=O.[Cs+].[Cs+].O>CN(C=O)C.CCOC(C)=O>[F:18][CH:17]([F:19])[CH2:16][O:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1참가 물질
7
실험 절차
A mixture of commercially available 4-hydroxybenzaldehyde (2.000 g; 16.40 mmol), 2,2-difluoroethyl trifluoromethanesulfonate (3.506 g; 16.40 mmol), and Cs2CO3 (8.004 g; 24.60 mmol) in anh. DMF (30 ml) was stirred at rt, under nitrogen, for 18 h. Water and AcOEt were added and the organic layer was washed with water, dried over anh. MgSO4, filtered, and concentrated to dryness under reduced pressure affording 4-(2,2-difluoroethoxy)benzaldehyde as an orange oil. LC-MS (conditions A): tR=0.65 min.; no ionisation.
후처리
- washthe organic layer was washed with water
- dry with materialdried over anh. MgSO4
- filtrationfiltered
- concentrationconcentrated to dryness under reduced pressure
출처 및 근거
- ORD 기록
- ord-d1ead4252f044122adf5abe54b4bafc0
- 출처 데이터셋
- uspto-grants-2016_01
- 특허 번호
- US09242970B2
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