Tetrahydrofuran → 2-Chloro-4-(3,3-dimethylbut-1-ynyl)benzoic acid
反応式
[Cl:1][C:2]1[CH:11]=[C:10]([C:12]#[C:13][C:14]([CH3:17])([CH3:16])[CH3:15])[CH:9]=[CH:8][C:3]=1[C:4]([O:6]C)=[O:5].[OH-].[Na+].C1COCC1>CO>[Cl:1][C:2]1[CH:11]=[C:10]([C:12]#[C:13][C:14]([CH3:17])([CH3:16])[CH3:15])[CH:9]=[CH:8][C:3]=1[C:4]([OH:6])=[O:5]参加物
5
実験手順
A mixture of methyl 2-chloro-4-(3,3-dimethylbut-1-ynyl)benzoate (330 mg, 0.0013 mol), 2N aq. NaOH (3.0 mL), THF (5 mL), and MeOH (5 mL) was stirred at rt for 5 h. The mixture was concentrated under vacuum and the residue was treated with water and acidified with 1N HCl to pH 2-3, and extracted with EtOAc. The organic layer was washed with brine, dried (Na2SO4), and concentrated under vacuum to give the product (305 mg, 98%) as a white solid. tR=3.56 min, 234.9 & 236.9 (M−1).
後処理
- concentrationThe mixture was concentrated under vacuum
- additionthe residue was treated with water
- extractionextracted with EtOAc
- washThe organic layer was washed with brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated under vacuum
出典と根拠
- ORDレコード
- ord-042bfefd9fa24c5db6c95ac365733173
- 出典データセット
- uspto-grants-2009_08
- 特許番号
- US07576099B2
反応ノート
読み込み中…