Acetic Anhydride → HCID 178472004、化合物
反応式
[F:1][C:2]1[C:15]([F:16])=[C:14]([F:17])[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].[CH3:19]C(OC(C)=O)=O.C(OCC)(OCC)OCC.[NH2:36][CH2:37][CH2:38][CH2:39][CH2:40][OH:41]>>[OH:41][CH2:40][CH2:39][CH2:38][CH2:37][NH:36][CH:19]=[C:6]([C:4](=[O:5])[C:3]1[CH:12]=[C:13]([F:18])[C:14]([F:17])=[C:15]([F:16])[C:2]=1[F:1])[C:7]([O:9][CH2:10][CH3:11])=[O:8]参加物
5
反応条件
- 温度
- 130 °C
実験手順
A mixture of ethyl 2,3,4,5-tetrafluorobenzoylacetate (2.64 g, 10.0 mmol), Ac2O (2.36 mL, 25.0 mmol) and triethyl orthoformate (2.49 mL, 15.0 mmol) was stirred at 130° C. for 3 h. The mixture was concentrated in vacuo and dried under high vacuum. The crude product was dissolved in EtOH (50 mL) and 4-amino-1-butanol (0.972 mL, 10.5 mmol) was added. After stirred at room temperature for 17 h, the mixture was concentrated in vacuo and the crude product was purified by column chromatography (Hexane:EtOAc 2:1→1:2) to yield ethyl 3-(4-hydroxybutylamino)-2-(2,3,4,5-tetrafluorobenzoyl)acrylate (3.53 g, 97%) as a pale yellow solid.
後処理
- concentrationThe mixture was concentrated in vacuo
- customdried under high vacuum
- dissolutionThe crude product was dissolved in EtOH (50 mL)
- stirringAfter stirred at room temperature for 17 h
- concentrationthe mixture was concentrated in vacuo
- customthe crude product was purified by column chromatography (Hexane:EtOAc 2:1→1:2)
出典と根拠
- ORDレコード
- ord-5fce5efe24684caaa2bfa9a38084cc0c
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08063221B2
反応ノート
読み込み中…