Acetic Anhydride → 4-Acetoxy-2,3-dimethyl-6-(4-trifluoromethoxyphenoxy)-7-trifluoromethyl-quinoline
반응식
[CH3:1][C:2]1[C:11]([CH3:12])=[C:10]([OH:13])[C:9]2[C:4](=[CH:5][C:6]([C:26]([F:29])([F:28])[F:27])=[C:7]([O:14][C:15]3[CH:20]=[CH:19][C:18]([O:21][C:22]([F:25])([F:24])[F:23])=[CH:17][CH:16]=3)[CH:8]=2)[N:3]=1.[C:30](OC(=O)C)(=[O:32])[CH3:31]>>[C:30]([O:13][C:10]1[C:9]2[C:4](=[CH:5][C:6]([C:26]([F:28])([F:29])[F:27])=[C:7]([O:14][C:15]3[CH:20]=[CH:19][C:18]([O:21][C:22]([F:23])([F:24])[F:25])=[CH:17][CH:16]=3)[CH:8]=2)[N:3]=[C:2]([CH3:1])[C:11]=1[CH3:12])(=[O:32])[CH3:31]참가 물질
3
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- 온도
- 122.5 °C
실험 절차
Acetic anhydride (40 mL) was added to 1.73 g of 2,3-dimethyl-4-hydroxy-6-(4-trifluoromethoxyphenoxy)-7-trifluoromethyl-quinoline obtained as crystals, and the mixture was heated at 120 to 125° C. for one hr. This reaction solution was concentrated under the reduced pressure, ethyl acetate was then added to the concentrate, and the mixture was washed with brine. Thereafter, the solvent was removed under the reduced pressure, and the crude product was purified by column chromatography on silica gel (BW300, manufactured by Fuji Sylysia Chemical Ltd., solvent: n-hexane/ethyl acetate) to give 0.82 g of 4-acetoxy-2,3-dimethyl-6-(4-trifluoromethoxyphenoxy)-7-trifluoromethyl-quinoline.
후처리
- customobtained as crystals
- concentrationThis reaction solution was concentrated under the reduced pressure, ethyl acetate
- additionwas then added to the concentrate
- washthe mixture was washed with brine
- customThereafter, the solvent was removed under the reduced pressure
- customthe crude product was purified by column chromatography on silica gel (BW300, manufactured by Fuji Sylysia Chemical Ltd., solvent: n-hexane/ethyl acetate)
출처 및 근거
- ORD 기록
- ord-d7bcd846516147a7ac62bcf04da4e391
- 출처 데이터셋
- uspto-grants-2011_02
- 특허 번호
- US07880006B2
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