Methyl iodide → methyl 4-chloro-2-formylbenzoate
反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=[O:11])[O:6][CH:5]2[OH:12].I[CH3:14]>ClCCl>[CH3:14][O:6][C:7](=[O:11])[C:8]1[CH:9]=[CH:10][C:2]([Cl:1])=[CH:3][C:4]=1[CH:5]=[O:12]参加物
4
実験手順
A solution of 5-chloro-3-hydroxy-3H-isobenzofuran-1-one (10 g, 54 mmol) and iodomethane (80 g, 560 mmol) in dichloromethane (200 mL) was heated at reflux, then the heating bath was removed. To the above solution was added triethylamine (60 g) at a rate that maintained a brisk reflux. After the addition was completed, the mixture was allowed to cool to room temperature and stirred for 72 h. The mixture was purified by column chromatography to give the title product (1.5 g).
後処理
- temperatureat reflux
- customthe heating bath was removed
- additionTo the above solution was added triethylamine (60 g) at a rate
- temperaturethat maintained a brisk reflux
- additionAfter the addition
- customThe mixture was purified by column chromatography
出典と根拠
- ORDレコード
- ord-e46004cb392f47538378463cd0c3cbb5
- 出典データセット
- uspto-grants-2009_02
- 特許番号
- US07495007B2
反応ノート
読み込み中…