Methanol → HCID 178501285、化合物
反応式
[OH:1][CH:2]1[CH2:7][CH2:6][CH:5]([C:8]([OH:10])=[O:9])[CH2:4][CH2:3]1.S(=O)(=O)(O)O.[CH3:16]O>>[OH:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([C:8]([O:10][CH3:16])=[O:9])[CH2:4][CH2:3]1参加物
4
反応条件
- 温度
- 60 °C
実験手順
A 250-mL round-bottom flask, purged and maintained with an inert atmosphere of nitrogen, was charged with 4-hydroxycyclohexane-1-carboxylic acid (15.7 g, 108.90 mmol, 1.00 equiv) in methanol (90 mL). Sulfuric acid (0.8 mL) was added to the mixture slowly. The resulting solution was stirred for 10 hr at 60° C. The reaction was then quenched by the addition of 200 mL of sodium bicarbonate (sat.). The resulting solution was extracted with 3×200 mL of ethyl acetate and the organic layers combined and dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting trans-methyl 4-hydroxycyclohexane-1-carboxylate (16.6 g, 96%) was obtained as a light yellow oil.
後処理
- customA 250-mL round-bottom flask, purged
- temperaturemaintained with an inert atmosphere of nitrogen
- customThe reaction was then quenched by the addition of 200 mL of sodium bicarbonate (sat.)
- extractionThe resulting solution was extracted with 3×200 mL of ethyl acetate
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-165ee679b3bb49bebe64baa402bdf67b
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09212190B2
反応ノート
読み込み中…