Water → 1,2-Benzenedimethanol
反応式
[C:1](O)(=[O:11])[C:2]1[C:3](=[CH:7][CH:8]=[CH:9][CH:10]=1)[C:4](O)=[O:5].[H-].[H-].[H-].[H-].[Li+].[Al+3].O.[OH-].[Na+]>C1COCC1>[C:2]1([CH2:1][OH:11])[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[CH2:4][OH:5]参加物
6
実験手順
A solution of phthalic acid (9 g, 0.05 mol) in anhydrous THF (200 mL) was added to LAH (7.6 g, 0.2 mol) in THF (250 mL) dropwise, and the mixture was refluxed for 18 hours. The mixture was cooled in ice bath and carefully added water dropwise, followed by 50% NaOH (150 mL), and then removed the ice bath added water slowly with stirring until the gray precipitate turns white. The mixture was filtrated and the filtrate was concentrated to give crude 1,2-phenylenedimethanol (7 g, 92%).
後処理
- temperaturethe mixture was refluxed for 18 hours
- temperatureThe mixture was cooled in ice bath
- customremoved the ice bath
- additionadded water slowly
- filtrationThe mixture was filtrated
- concentrationthe filtrate was concentrated
出典と根拠
- ORDレコード
- ord-0b8e32ae7fa243aebe9cca9c6f902b45
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08633212B2
反応ノート
読み込み中…