Triethylamine → 4-Bromo-2,6-difluorobenzaldehyde
反応式
[Br:1][C:2]1[CH:9]=[C:8]([F:10])[C:5]([CH2:6][OH:7])=[C:4]([F:11])[CH:3]=1.C(N(CC)CC)C>C(Cl)Cl.CS(C)=O.CCOCC>[Br:1][C:2]1[CH:3]=[C:4]([F:11])[C:5]([CH:6]=[O:7])=[C:8]([F:10])[CH:9]=1参加物
6
実験手順
To a solution of 4-bromo-2,6-difluorobenzylalcohol (0.200 g, 0.9 mmol) in DCM (4 ml) and DMSO (0.440 ml) was added triethylamine (1 ml, 0.72 mmol) and sulfur trioxide pyridine complex (0.570 g, 3.6 mmol) and the resulting solution was stirred at room temperature for 3 hours. The solution was diluted with Et2O and washed with 0.5M aqueous HCl, 1M sodium bicarbonate solution and brine. The organic phase was dried over MgSO4 and the solvent removed in vacuo to afford 4-bromo-2,6-difluorobenzaldehyde (0.166 g, 0.75 mmol, 84%) as a white solid. 1H NMR (CDCl3) δ 7.22 (2H, d), 10.29 (1H, br. s). LCMS (2) Rt: 2.74 min.
後処理
- washwashed with 0.5M aqueous HCl, 1M sodium bicarbonate solution and brine
- dry with materialThe organic phase was dried over MgSO4
- customthe solvent removed in vacuo
出典と根拠
- ORDレコード
- ord-722468b6c01a423f988487eb31c55f56
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08378095B2
反応ノート
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