Sulfuric Acid → 2-(Acetyloxy)-5-chlorobenzoic acid

HRID 644392

反応式

HRID 644392 の反応式
S(=O)(=O)(O)O.[Cl:6][C:7]1[CH:15]=[C:11]([C:12]([OH:14])=[O:13])[C:10]([OH:16])=[CH:9][CH:8]=1.[C:17](OC(=O)C)(=[O:19])[CH3:18]>>[C:17]([O:16][C:10]1[CH:9]=[CH:8][C:7]([Cl:6])=[CH:15][C:11]=1[C:12]([OH:14])=[O:13])(=[O:19])[CH3:18]

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 94475-Chlorosalicylic Acid

生成物 1

HCID 28208132-(Acetyloxy)-5-chlorobenzoic acid収率 93%

実験手順

Concentrated sulfuric acid (0.08 mL) was added slowly to a mixture of 5-chlorosalicylic acid (13.35 g, 77 mmol) and acetic anhydride (20 mL). After the reaction mixture was solidified, it was poured into ice water and extracted with ethyl acetate. The organic layer was washed with water and brine, and dried over anhydrous sodium sulfate. The residue obtained by evaporation of the solvent under reduced pressure was washed with n-hexane under suspension to give the title compound (15.44 g, 93.0%) as a white crystal.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe residue obtained by evaporation of the solvent under reduced pressure
  5. washwas washed with n-hexane under suspension

出典と根拠

ORDレコード
ord-f31a00664c4e479686f57363ead5e31a
出典データセット
uspto-grants-2010_04
特許番号
US07700655B2

関連ノート

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