Sodium Hydroxide → 6-Methylsalicylic Acid
反応式
[OH:1][C:2]1[CH:12]=[CH:11][CH:10]=[C:9]([CH3:13])[C:3]=1[C:4]([O:6]CC)=[O:5].[OH-].[Na+]>CO>[OH:1][C:2]1[CH:12]=[CH:11][CH:10]=[C:9]([CH3:13])[C:3]=1[C:4]([OH:6])=[O:5]参加物
4
実験手順
Step 1 A solution of ethyl 2-hydroxy-6-methylbenzoate (2.04 g, 11.32 mmol) in methanol (25 mL) was treated at rt with 1 M aqueous sodium hydroxide (45.3 mL, 45.3 mmol) and the mixture was heated at reflux for 6 h. The mixture was cooled to rt and the methanol was removed under vacuum. The aqueous residue was treated with 1 M hydrochloric acid to pH ca. 1. The precipitate was collected by filtration, washed with water and dried under vacuum to give 2-hydroxy-6-methylbenzoic acid as a white solid (1.62 g, 94%). 1H NMR (400 MHz, methanol-d4) δ 7.26 (1H, t, J=7.92 Hz), 6.75 (2H, t, J=7.92 Hz), 2.55 (3H, s). Mass spectrum m/z 153.1 (M+H)+.
後処理
- temperaturethe mixture was heated
- temperatureat reflux for 6 h
- customthe methanol was removed under vacuum
- additionThe aqueous residue was treated with 1 M hydrochloric acid to pH ca. 1
- filtrationThe precipitate was collected by filtration
- washwashed with water
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-709b799f5b24458fb9a3771a4f98b731
- 出典データセット
- uspto-grants-2011_12
- 特許番号
- US08084620B2
反応ノート
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