Lithium Hydroxide → 4-(Dimethylcarbamoyl)benzoic acid
反応式
[CH3:1][N:2]([CH3:15])[C:3]([C:5]1[CH:14]=[CH:13][C:8]([C:9]([O:11]C)=[O:10])=[CH:7][CH:6]=1)=[O:4].[Li+].[OH-]>CO>[CH3:1][N:2]([CH3:15])[C:3]([C:5]1[CH:14]=[CH:13][C:8]([C:9]([OH:11])=[O:10])=[CH:7][CH:6]=1)=[O:4]参加物
4
実験手順
To a soln. of methyl 4-(dimethylcarbamoyl)benzoate (100 mg, 0.483 mmol, crude from above preparation) in MeOH (4 ml) was added LiOH (1 ml, 3.00 mmol). The mixture was stirred at r.t for 1.5 hrs. Evaporated to remove the solvent. The residue was dissolved in water (3 ml), neutralized w/6M HCl to PH=3, extracted w/EtOAc (3×). The combined organic layer was dried (Na2SO4) and evaporated to afford 4-(dimethylcarbamoyl)benzoic acid (64 mg, 0.315 mmol, 65.2% yield) as solid, which was used for the next reaction directly.
後処理
- customEvaporated
- customto remove the solvent
- dissolutionThe residue was dissolved in water (3 ml)
- extractionextracted w/EtOAc (3×)
- dry with materialThe combined organic layer was dried (Na2SO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-4a2e2d5c01b04df38d879fb7694bd8cd
- 出典データセット
- uspto-grants-2013_01
- 特許番号
- US08362004B2
反応ノート
読み込み中…