Water → 3-Chlorobenzocyclobutene-1-carboxylic acid
反応式
[Cl:1][C:2]1[C:9]2[CH2:8][CH:7]([C:10]#N)[C:6]=2[CH:5]=[CH:4][CH:3]=1.[OH-:12].[K+].[OH2:14]>C(O)C>[Cl:1][C:2]1[C:9]2[CH:8]=[C:7]([C:10]([OH:14])=[O:12])[C:6]=2[CH:5]=[CH:4][CH:3]=1参加物
5
実験手順
5.0 g of 3-chloro-1-cyanobenzocyclobutane (prepared according to the process described in Patent EP 119,107) are added to a solution of 6.0 g of potassium hydroxide in 58 ml of ethanol The mixture is stirred at room temperature overnight. 7.5 ml of water are then added and the mixture is heated to reflux for 6 hours. The ethanol is evaporated off to dryness. The residue is taken up with water and the aqueous phase is washed with ethyl ether, then acidified (pH 1) with 1N hydrochloric acid and extracted with dichloromethane. The organic phase is dried, filtered and evaporated to dryness.
後処理
- temperaturethe mixture is heated
- temperatureto reflux for 6 hours
- customThe ethanol is evaporated off to dryness
- washthe aqueous phase is washed with ethyl ether
- extractionextracted with dichloromethane
- customThe organic phase is dried
- filtrationfiltered
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-68c27c083a2b4eb591ad0a191d200ae5
- 出典データセット
- uspto-grants-1992_07
- 特許番号
- US05134147
反応ノート
読み込み中…