反応式
[F:1][C:2]1[C:15]([F:16])=[C:14](F)[C:13]([F:18])=[CH:12][C:3]=1[C:4]([CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5].[CH2:19]([O:21][C:22]([N:24]([CH2:26][CH:27]1[O:32][CH2:31][CH2:30][NH:29][CH2:28]1)[CH3:25])=[O:23])[CH3:20].C(=O)([O-])O.[Na+]>C(#N)C>[CH2:19]([O:21][C:22]([N:24]([CH2:26][CH:27]1[CH2:28][N:29]([C:14]2[C:13]([F:18])=[CH:12][C:3]([C:4]([CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5])=[C:2]([F:1])[C:15]=2[F:16])[CH2:30][CH2:31][O:32]1)[CH3:25])=[O:23])[CH3:20]参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
A suspension of 26.4 g of ethyl 2,3,4,5-tetrafluorobenzoylacetate, 18.7 g of 2-(N-ethoxycarbonyl-N-methylaminomethyl)morpholine and 8.4 g of sodium hydrogen carbonate in 130 ml of acetonitrile is refluxed for 7 hours. The reaction mixture is concentrated under reduced pressure, to the obtained residue is added 100 ml of chloroform and the solution is washed with water. After drying over anhydrous magnesium sulfate, the chloroform is distilled off under reduced pressure and the residue is purified by chromatography on silica gel to give 30.0 g of ethyl 4-[2-(N-ethoxycarbonyl-N-methylaminomethyl)morpholino]-2,3,5-trifluorobenzoylacetate in 67% yield, as an oily substance.
後処理
- temperatureis refluxed for 7 hours
- concentrationThe reaction mixture is concentrated under reduced pressure, to the obtained residue
- additionis added 100 ml of chloroform
- washthe solution is washed with water
- dry with materialAfter drying over anhydrous magnesium sulfate
- distillationthe chloroform is distilled off under reduced pressure
- customthe residue is purified by chromatography on silica gel
出典と根拠
- ORDレコード
- ord-b97f01db4b1f4bc4a7713f5077875784
- 出典データセット
- uspto-grants-1989_12
- 特許番号
- US04889857
関連ノート
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