反応式
[CH2:1]([N:3]([CH2:9][CH3:10])[CH:4]1[CH2:8][CH2:7][NH:6][CH2:5]1)[CH3:2].[CH2:11]([O:13][C:14](=[O:24])[C:15]([C:17]1[CH:22]=[CH:21][C:20]([Br:23])=[CH:19][CH:18]=1)=[CH2:16])[CH3:12]>C1COCC1>[CH2:11]([O:13][C:14](=[O:24])[CH:15]([C:17]1[CH:18]=[CH:19][C:20]([Br:23])=[CH:21][CH:22]=1)[CH2:16][N:6]1[CH2:7][CH2:8][CH:4]([N:3]([CH2:9][CH3:10])[CH2:1][CH3:2])[CH2:5]1)[CH3:12]参加物
4
実験手順
To a solution of diethyl-pyrrolidin-3-yl-amine (0.685 g, 6 mmol) in THF (10 mL) was added 2-(4-bromo-phenyl)-acrylic acid ethyl ester (1.27 g, 5 mmol) dropwise in THF at 0 degrees Celsius. Then the mixture was stirred at room temperature for 1 h and concentrated in vacuo. The residue was dissolved in EtOAc (30 mL), washed with water (20 mL×2), brine, dried over Na2SO4, filtered and evaporated. The obtained oil was used directly without further purification. MS: calc'd 397 (MH+), exp 397 (MH+).
後処理
- concentrationconcentrated in vacuo
- dissolutionThe residue was dissolved in EtOAc (30 mL)
- washwashed with water (20 mL×2), brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated
- customThe obtained oil was used directly without further purification
出典と根拠
- ORDレコード
- ord-d6f463bfc9244d15b6edf63ba213c07a
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08202866B2
関連ノート
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