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[F:1][C:2]([F:14])([F:13])[O:3][C:4]1[CH:12]=[CH:11][C:7]([CH:8]=[N:9][OH:10])=[CH:6][CH:5]=1.[Cl:15]N1C(=O)CCC1=O>CN(C=O)C>[OH:10]/[N:9]=[C:8](\[Cl:15])/[C:7]1[CH:11]=[CH:12][C:4]([O:3][C:2]([F:13])([F:14])[F:1])=[CH:5][CH:6]=1참가 물질
4
실험 절차
To a solution of 4-(trifluoromethoxy)benzaldehyde oxime (9.5 g, 46 mmol) in DMF (80 ml) was added N-chlorosuccinimide (8.0 g, 60 mmol) and the resulting mixture was stirred at RT for 5 h. The volatiles were removed under reduced pressure and the residue was dissolved in EtOAc, and washed with H2O, brine. The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure. The solid residue was used without further purification for the following step. 1H NMR (500 MHz, CDCl3) δ 7.78 (d, J=7.2 Hz, 2H), 7.13 (d, J=6.8 Hz, 2H).
후처리
- customThe volatiles were removed under reduced pressure
- dissolutionthe residue was dissolved in EtOAc
- washwashed with H2O, brine
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe solid residue was used without further purification for the following step
출처 및 근거
- ORD 기록
- ord-99c499aaafe343a1b83f74cf70c68bc8
- 출처 데이터셋
- uspto-grants-2015_04
- 특허 번호
- US09018380B2
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