反応式
[C:1](O)(=O)C.CO.[P].C[O:9][C:10]1[CH:15]=[CH:14][C:13]([CH:16]([CH3:20])[C:17]([OH:19])=[O:18])=[CH:12][CH:11]=1>I>[OH:9][C:10]1[CH:15]=[CH:14][C:13]([CH:16]([CH3:20])[C:17]([O:19][CH3:1])=[O:18])=[CH:12][CH:11]=1参加物
6
実験手順
In a mixture of 12ml of hydroiodic acid, 90ml of acetic acid and 1g of phosphorus 10g of 2-(4-methoxyphenyl)propionic acid was refluxed for 3 hours and the reaction mixture was concentrated. 20ml of methanol and 2ml of sulfuric acid were added to the residue and the mixture was refluxed for one hour. After the methanol was concentrated, the water was added to the residue and extracted with ether. The extract was washed over magnesium sulfate and the ether was distilled off. The residue was distilled under reduced pressure to give the object compound having b.p. 150° - 153° C/6mm Hg in a yield of 6.7g (67%)
後処理
- temperaturewas refluxed for 3 hours
- concentrationthe reaction mixture was concentrated
- addition20ml of methanol and 2ml of sulfuric acid were added to the residue
- temperaturethe mixture was refluxed for one hour
- concentrationAfter the methanol was concentrated
- additionthe water was added to the residue
- extractionextracted with ether
- washThe extract was washed over magnesium sulfate
- distillationthe ether was distilled off
- distillationThe residue was distilled under reduced pressure
- customto give the object compound
出典と根拠
- ORDレコード
- ord-bae7d0942c714db0bf3630cafccbeb6d
- 出典データセット
- uspto-grants-1977_04
- 特許番号
- US04016193
関連ノート
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