Sodium Hydroxide → 3-Methyl-1-benzofuran-5-carboxylic acid
反応式
[CH3:1][C:2]1[C:6]2[CH:7]=[C:8]([C:11]([O:13]C)=[O:12])[CH:9]=[CH:10][C:5]=2[O:4][CH:3]=1.[OH-].[Na+]>CO.O>[CH3:1][C:2]1[C:6]2[CH:7]=[C:8]([C:11]([OH:13])=[O:12])[CH:9]=[CH:10][C:5]=2[O:4][CH:3]=1参加物
5
実験手順
Methyl 3-methyl-1-benzofuran-5-carboxylate (365 mg, 1.9 mmol) is dissolved in MeOH (7 mL), diluted with H2O (3.5 mL) and treated with 3N NaOH (1.41 mL, 4.2 mmol). The mixture is diluted with MeOH (3.5 mL) to homogeneity, stirred at RT for 2.5 days then concentrated to dryness. The residue is dissolved in H2O (5 mL) and acidified to pH 2 with concentrated HCl. The resulting solid is filtered and dried in a vacuum oven at 40° C. for 18 h to afford 321 mg (95%) of 3-methyl-1-benzofuran-5-carboxylic acid as a white solid. HRMS (FAB) calcd for C10H8O3+H: 177.0552, found: 177.0553 (M+H)+.
後処理
- concentrationthen concentrated to dryness
- dissolutionThe residue is dissolved in H2O (5 mL)
- filtrationThe resulting solid is filtered
- customdried in a vacuum oven at 40° C. for 18 h
出典と根拠
- ORDレコード
- ord-379062f285a94a91a6b87e4c0ba0ca87
- 出典データセット
- uspto-grants-2005_05
- 特許番号
- US06894042B2
反応ノート
読み込み中…