Sodium Bicarbonate → 4-Chloro-2-formylbenzoic acid
反応式
[CH:1]([C:3]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:4]=1[C:5](NC)=[O:6])=[O:2].C(=O)([O-])[OH:15].[Na+]>Cl>[CH:1]([C:3]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:4]=1[C:5]([OH:15])=[O:6])=[O:2]参加物
4
実験手順
A mixture of 2-formyl-4-chloro-N-methylbenzamide (3.19 g) and 10M hydrochloric acid (30 ml) was heated at reflux for 18 hours. The mixture was cooled and basified with saturated sodium hydrogen carbonate solution. The solution was then washed with ethyl acetate, then acidified with 2M hydrochloric acid. The product was extracted with ethyl acetate and the combined extracts dried with magnesium sulfate. The solution was then filtered and concentrated. This furnished 2-formyl-4-chlorobenzoic acid as a yellow solid (2.22 g, 75%); 1H NMR (400 MHz, CDCl3) δ 6.65 (0.5H, brs), 7.50 (2H, m), 7.65 (1H, m), 7.85 (0.5H, brm), 8.05 (1H, m).
後処理
- temperaturewas heated
- temperatureat reflux for 18 hours
- temperatureThe mixture was cooled
- washThe solution was then washed with ethyl acetate
- extractionThe product was extracted with ethyl acetate
- dry with materialthe combined extracts dried with magnesium sulfate
- filtrationThe solution was then filtered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-47d04d663d25480da1531e63c71b2b25
- 出典データセット
- uspto-grants-2011_12
- 特許番号
- US08071618B2
反応ノート
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