Methyl iodide → methyl 3-fluoro-2-formylbenzoate
反応式
[F:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]([OH:12])[O:5][C:6]2=[O:7].[C:13](=O)([O-])[O-].[K+].[K+].CI>CC(C)=O>[F:1][C:2]1[C:3]([CH:4]=[O:12])=[C:8]([CH:9]=[CH:10][CH:11]=1)[C:6]([O:5][CH3:13])=[O:7]参加物
5
実験手順
A stirred mixture containing 7.36 g 4-fluoro-3-hydroxyphthalide, 18.15 g potassium carbonate and 11 mL methyl iodide in 125 mL acetone is heated at reflux for two hours. After stirring overnight at room temperature, the mixture is filtered and concentrated. The residue is dispersed in 200 mL ether, filtered and the filtrate concentrated to give 7.6 g residue which is used directly without further purification. The nmr spectrum of this material is consistent with that expected for the desired product.
後処理
- temperatureis heated
- temperatureat reflux for two hours
- filtrationthe mixture is filtered
- concentrationconcentrated
- additionThe residue is dispersed in 200 mL ether
- filtrationfiltered
- concentrationthe filtrate concentrated
出典と根拠
- ORDレコード
- ord-39d89443bea04959ac5d2f4d9021f4e1
- 出典データセット
- uspto-grants-1986_08
- 特許番号
- US04608079
反応ノート
読み込み中…