Hydrochloric Acid → 2,4-Dimethoxybenzoic acid

HRID 501785

反応式

HRID 501785 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[CH:9][C:4]=1[C:5]([O:7]C)=[O:6].C(Cl)(Cl)Cl.O.Cl>C(O)C.[OH-].[Na+]>[CH3:1][O:2][C:3]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[CH:9][C:4]=1[C:5]([OH:7])=[O:6]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 6212ChloroformHCID 137451Benzoic acid, 2,4-dimethoxy-, methyl ester

生成物 1

HCID 70522,4-Dimethoxybenzoic acid収率 91.4%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 14798Sodium Hydroxide溶媒

反応条件

温度
32.5 °C

実験手順

53 g of methyl 2,4-dimethoxybenzoate was dissolved in 160 mL of ethanol, to which 104 mL of a 5M aqueous solution of sodium hydroxide was added, and this mixture was stirred for 2 hours at 25 to 40° C. Then, chloroform and water were added to the reaction mixture, which was adjusted to pH 2 with 6M hydrochloric acid, and then the organic phase was separated therefrom. After the resultant organic phase was washed with water and a saturated sodium chloride solution successively, the washed phase was dried over anhydrous magnesium sulfate, and the solvent was distilled out under reduced pressure to yield 45 g of 2,4-dimethoxybenzoic acid as white solid.

後処理

  1. additionwas added
  2. customthe organic phase was separated
  3. washAfter the resultant organic phase was washed with water
  4. dry with materiala saturated sodium chloride solution successively, the washed phase was dried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled out under reduced pressure

出典と根拠

ORDレコード
ord-e242f1be75104dde819827f3f1c9954d
出典データセット
uspto-grants-2010_08
特許番号
US07772285B2

関連ノート

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