Hydrochloric Acid → HCID 10198445、化合物
反応式
[Cl-].[Al+3].[Cl-].[Cl-].[C:5]1(=[O:11])[O:10][C:8](=O)[CH2:7][CH2:6]1.C([O:15][C:16]1[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH:17]=1)(=O)C.Cl.[N+](C)([O-])=[O:26]>>[O:26]=[C:21]1[CH2:22][CH2:23][C:16](=[O:15])[CH:20]1[CH2:19][CH2:18][CH2:17][CH2:8][CH2:7][CH2:6][C:5]([OH:10])=[O:11]参加物
実験手順
To a solution of 2.7 g of aluminum chloride in 15 ml of nitromethane, 1.0 g of succinic anhydride was added, and then 1.7 g of 1-cyclooctenyl acetate was added dropwise under cooling. The resultant mixture was stirred at room temperature overnight and refluxed with stirring for four hours. The mixture was cooled, poured into 50 ml of 1N hydrochloric acid containing ice, and extracted four times with 30 ml of ethyl acetate. The organic layer was extracted twice with 30 ml of a saturated aqueous sodium bicarbonate solution. The aqueous layer was washed with ethyl acetate at pH 7. The aqueous was adjusted to pH 2 with 6N hydrochloric acid, and again extracted four times with 30 ml of ethyl acetate. The extract was dried and concentrated. The residue was washed with water to give 0.2 g of 7-(2,5-dioxocyclopentyl) heptanoic acid. This product had a melting point of 105° to 122° C.
後処理
- temperatureunder cooling
- temperaturerefluxed
- temperatureThe mixture was cooled
- additioncontaining ice
- extractionextracted four times with 30 ml of ethyl acetate
- extractionThe organic layer was extracted twice with 30 ml of a saturated aqueous sodium bicarbonate solution
- washThe aqueous layer was washed with ethyl acetate at pH 7
- extractionagain extracted four times with 30 ml of ethyl acetate
- customThe extract was dried
- concentrationconcentrated
- washThe residue was washed with water
出典と根拠
- ORDレコード
- ord-bc84cc9f939f471da520bb265e00cb7e
- 出典データセット
- uspto-grants-1989_07
- 特許番号
- US04849535
反応ノート
読み込み中…