Tetrahydrofuran → HCID 178449877、化合物
反応式
[F:1][C:2]([F:13])([F:12])[CH2:3][O:4][C:5]1[CH:11]=[CH:10][C:8]([NH2:9])=[CH:7][CH:6]=1.C([N:16]([CH2:19][CH3:20])CC)C.[CH2:21]1COC[CH2:22]1.C(OCC)(=O)C>O>[F:1][C:2]([F:12])([F:13])[CH2:3][O:4][C:5]1[CH:11]=[CH:10][C:8]([NH:9][C:19](=[NH:16])[CH2:20][CH2:21][CH3:22])=[CH:7][CH:6]=1参加物
6
反応条件
- 温度
- 70 °C
実験手順
A mixture of ethyl butylimidate hydrochloride (10.0 g), 4-(2,2,2-trifluoroethoxy)aniline (12.6 g), triethylamine (6.67 g) and THF (250 mL) was stirred at 70° C. for 2 days. To the reaction mixture were added ethyl acetate and water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to aminopropylsilane-bonded silica gel column chromatography (ethyl acetate/hexane) to give the title compound (4.80 g) as a solid.
後処理
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with saturated brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-0af3bb64acb847fab8f831589a93f56d
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09023858B2
反応ノート
読み込み中…