Formic Acid → N-[4-methoxy-3-(trifluoromethyl)benzyl]formamide
반응식
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[CH:6]=O.[CH:15]([NH2:17])=[O:16].C(O)=O.O>C(OCC)(=O)C>[CH3:12][O:11][C:10]1[CH:9]=[CH:8][C:5]([CH2:6][NH:17][CH:15]=[O:16])=[CH:4][C:3]=1[C:2]([F:14])([F:13])[F:1]참가 물질
6
반응 조건
- 온도
- 130 °C
실험 절차
A mixture of 5.8 g 3-trifluoromethyl-p-anisaldehyde, 8.6 ml formamide, and 13.6 ml formic acid was stirred at 130° C. for 9 hr. After cooling, water and ethyl acetate were added thereto. The ethyl acetate layer was recovered and washed with brine. It was dried over anhydrous magnesium sulfate, filtered, and evaporated. The resulting residue was purified by silica gel column chromatography to give 3.8 g of N-[4-methoxy-3-(trifluoromethyl)benzyl]formamide.
후처리
- temperatureAfter cooling
- customThe ethyl acetate layer was recovered
- washwashed with brine
- dry with materialIt was dried over anhydrous magnesium sulfate
- filtrationfiltered
- customevaporated
- customThe resulting residue was purified by silica gel column chromatography
출처 및 근거
- ORD 기록
- ord-6687c211faa74f90ad4a2435468d95bf
- 출처 데이터셋
- uspto-grants-2002_12
- 특허 번호
- US06498159B1
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