Sodium Hydroxide → 1-methyl-1H-1,2,3-triazole-5-carboxylic acid
反応式
[CH3:1][N:2]1[C:6]([CH:7]=[O:8])=[CH:5][N:4]=[N:3]1.[OH-].[Na+].[Mn]([O-])(=O)(=O)=[O:12].[K+]>O>[CH3:1][N:2]1[C:6]([C:7]([OH:12])=[O:8])=[CH:5][N:4]=[N:3]1参加物
5
実験手順
To a solution of 1-methyl-1H-1,2,3-triazole-5-carbaldehyde (Preparation 33, 5 g, 45 mmol) and sodium hydroxide (8.59 g, 215 mmol) in water (120 ml) at 15° C. was added dropwise a solution of potassium permanganate (5.83 g, 36.9 mmol) in water (120 ml). The reaction was stirred at room temperature for 30 minutes and then heated to reflux for 1 hour. The reaction was filtered and the filtrate acidified to pH 3 with concentrated HCl before extracting with ethyl acetate (3×100 ml). The combined organic extracts were washed with saturated aqueous brine, dried over Na2SO4 and concentrated in vacuo to afford the title compound.
後処理
- temperatureheated
- temperatureto reflux for 1 hour
- filtrationThe reaction was filtered
- extractionbefore extracting with ethyl acetate (3×100 ml)
- washThe combined organic extracts were washed with saturated aqueous brine
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-73a70a38c7384a2fbac89c9ab3660e9d
- 出典データセット
- uspto-grants-2012_03
- 特許番号
- US08134007B2
反応ノート
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