Acetic Anhydride → 4-Acetoxy-2,3-dimethyl-6-(4-trifluoromethoxyphenoxy)-7-trifluoromethyl-quinoline
反応式
[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]参加物
3
反応条件
- 温度
- 122.5 °C
実験手順
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.
後処理
- 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)
出典と根拠
- ORDレコード
- ord-d7bcd846516147a7ac62bcf04da4e391
- 出典データセット
- uspto-grants-2011_02
- 特許番号
- US07880006B2
反応ノート
読み込み中…