Triethylamine → 4-Bromo-2,6-difluorobenzaldehyde
반응식
[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]=1참가 물질
6
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-722468b6c01a423f988487eb31c55f56
- 출처 데이터셋
- uspto-grants-2013_02
- 특허 번호
- US08378095B2
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