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Sodium Bicarbonate → 4-Chloro-2-formylbenzoic acid

HRID 1091432
ノート
印刷プレビュー

反応式

HRID 1091432 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 516892Sodium BicarbonateHCID 577253672-formyl-4-chloro-N-methylbenzamide

生成物 1

HCID 110414214-Chloro-2-formylbenzoic acid

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

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) ppm.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 18 hours
  3. temperatureThe mixture was cooled
  4. washThe solution was then washed with ethyl acetate
  5. extractionThe product was extracted with ethyl acetate
  6. dry with materialthe combined extracts dried with magnesium sulfate
  7. filtrationThe solution was then filtered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-8fb073b120494067b7563b80fda7c1b0
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08129381B2

反応ノート

読み込み中…