Ethyl Acetate → 2,3-Dihydro-1,4-benzothiazine
反応式
[S:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[NH:4][C:3](=O)[CH2:2]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].C(OCC)(=O)C>O1CCCC1>[S:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[NH:4][CH2:3][CH2:2]1参加物
5
実験手順
A solution of (2H)1,4-benzothiazin-3(4H)-one (20.0 g, 121.1 mmol) in anhydrous tetrahydrofuran (100 mL) was added to a stirred suspension of lithium aluminum hydride in anhydrous tetrahydrofuran (80 mL) under nitrogen at 0° C. The mixture was heated at reflux for 2 hrs and then poured into a mixture of ethyl acetate (300 mL) and ice (500 g). The organic layer was separated and the aqueous layer extracted with ethyl acetate. The combined organic layer was dried and concentrated under reduced pressure to provide 17.68 g (96.5%) of the desired compound which was used without further purification.
後処理
- temperatureThe mixture was heated
- temperatureat reflux for 2 hrs
- customThe organic layer was separated
- extractionthe aqueous layer extracted with ethyl acetate
- customThe combined organic layer was dried
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-75c8e7adbdc94062972659bb58dc2fe8
- 出典データセット
- uspto-grants-2004_06
- 特許番号
- US06743785B2
反応ノート
読み込み中…