Hydrochloric Acid → Benzoic acid, 3-fluoro-, methyl ester

HRID 128478

反応式

HRID 128478 の反応式
Cl.[F:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([OH:8])=[O:7].[CH3:12]O>>[F:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([O:8][CH3:12])=[O:7]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 99683-Fluorobenzoic Acid

生成物 1

HCID 521184Benzoic acid, 3-fluoro-, methyl ester収率 75%

実験手順

To a solution of anhydrous hydrochloric acid (10.5 g) in anhydrous methanol (100 ml) is added m-fluorobenzoic acid (13.3 g.; 0.095 mole). The reaction mixture is stirred at room temperature overnight. The solvent and anhydrous hydrochloric acid are then removed under vacuum and the residue slurried with hexane (100 ml). The hexane insoluble layer is decanted and the hexane solution water washed (2×100 ml) before drying with anhydrous magnesium sulfate. The hexane filtrate is then concentrated under vacuum to afford 11.0 g (75% yield) of methyl 3-fluorobenzoate as a yellow liquid. Elemental anal. calcd. for C8H7FO2 : C, 62.35; H, 4.57; F, 12.33. Found: C, 62.52; H, 4.70; F, 11.89.

後処理

  1. customThe solvent and anhydrous hydrochloric acid are then removed under vacuum
  2. customThe hexane insoluble layer is decanted
  3. washthe hexane solution water washed (2×100 ml)
  4. dry with materialbefore drying with anhydrous magnesium sulfate
  5. concentrationThe hexane filtrate is then concentrated under vacuum

出典と根拠

ORDレコード
ord-6684b72e7f404fc89f43475d0749ed83
出典データセット
uspto-grants-1981_03
特許番号
US04259510

関連ノート

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