4-Hydroxybenzaldehyde → 4-(2,2-Difluoroethoxy)benzaldehyde
反応式
[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]=1参加物
7
実験手順
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.
後処理
- washthe organic layer was washed with water
- dry with materialdried over anh. MgSO4
- filtrationfiltered
- concentrationconcentrated to dryness under reduced pressure
出典と根拠
- ORDレコード
- ord-d1ead4252f044122adf5abe54b4bafc0
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09242970B2
反応ノート
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