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Ethanol → HCID 54141100、化合物

HRID 266578
ノート
印刷プレビュー

反応式

HRID 266578 の反応式
[OH-].[Na+].[Cl:3][C:4]1[CH:13]=[CH:12][C:7]([C:8]([O:10]C)=[O:9])=[C:6]([S:14][CH3:15])[C:5]=1[C:16]([CH3:18])=[CH2:17].C(O)C>O>[Cl:3][C:4]1[CH:13]=[CH:12][C:7]([C:8]([OH:10])=[O:9])=[C:6]([S:14][CH3:15])[C:5]=1[C:16]([CH3:18])=[CH2:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 53939773HCID 53939773、化合物

生成物 1

HCID 54141100HCID 54141100、化合物収率 89.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of sodium hydroxide (7.0 g) in water was added to methyl 4-chloro-3-isopropenyl-2-(methylsulphenyl)benzoate (7.3 g) and the resulting mixture was heated at reflux for 2 hours. Ethanol was added and the mixture was heated at reflux for 1 hour. The ethanol was removed by evaporation and the aqueous residue was acidified to pH 1. It was extracted with ethyl acetate, washed with water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness to give 4-chloro-3-isopropenyl-2-(methylsulphenyl)benzoic acid (6.15 g) NMR (CDCl3) 2.05 (s,3H), 2.4 (s,3H), 4.85 (s, 1H), 5.35 (s,1H), 7.45 (d,1H), 7.85 (d,1H).

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureat reflux for 2 hours
  3. temperaturethe mixture was heated
  4. temperatureat reflux for 1 hour
  5. customThe ethanol was removed by evaporation
  6. extractionIt was extracted with ethyl acetate
  7. washwashed with water
  8. dry with materialdried (MgSO4)
  9. filtrationfiltered
  10. customThe filtrate was evaporated to dryness

出典と根拠

ORDレコード
ord-11506b33c1a84165bcab661f04aab200
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05650533

反応ノート

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