Sodium Azide → 4H-Pyran-4-one, 2-(azidomethyl)-5-hydroxy-
反応式
Cl[CH2:2][C:3]1[O:4][CH:5]=[C:6]([OH:10])[C:7](=[O:9])[CH:8]=1.[N-:11]=[N+:12]=[N-:13].[Na+]>CN(C=O)C.O>[N:11]([CH2:2][C:3]1[O:4][CH:5]=[C:6]([OH:10])[C:7](=[O:9])[CH:8]=1)=[N+:12]=[N-:13]参加物
5
実験手順
To a stirred solution of 2-chloromethyl-5-hydroxy-pyran-4-one (2) (105.0 g, 656.2 mmol) in DMF (600 mL) was added NaN3 (55.45 g, 853.12 mmol) and the reaction mixture was stirred at room temperature for 16 h. After completion of the reaction, the reaction mixture was diluted with water and extracted with ethyl acetate. Then, the combined organic layer was washed with water and brine, and dried over Na2SO4 and concentrated under reduced pressure to get 2-azidomethyl-5-hydroxy-pyran-4-one (3) (70.0 g, 63.83%) as a light brown solid.
後処理
- customAfter completion of the reaction
- extractionextracted with ethyl acetate
- washThen, the combined organic layer was washed with water and brine
- dry with materialdried over Na2SO4
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-81f0c4cd7323465da561f644963da6d7
- 出典データセット
- uspto-grants-2015_02
- 特許番号
- US08952039B2
反応ノート
読み込み中…