Hydrochloric Acid → 1-Benzofuran-3-carboxylic acid

HRID 1091312ノート

反応式

HRID 1091312 の反応式
CO.C[O:4][C:5]([C:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[O:9][CH:8]=1)=[O:6].[OH-].[Li+].Cl>O>[O:9]1[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[C:7]([C:5]([OH:6])=[O:4])=[CH:8]1

参加物

6

反応物 4

HCID 313Hydrochloric Acid2 回HCID 887MethanolHCID 3939Lithium HydroxideHCID 127770993-Benzofurancarboxylic acid, methyl ester

生成物 1

HCID 5956551-Benzofuran-3-carboxylic acid収率 91.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a methanol (30 mL) solution of 1-benzofuran-3-carboxylic acid methyl ester (5.25 g, 29.8 mmol) tetrahydrofuran (60 mL), water (30 mL) and lithium hydroxide (2.50 g, 59.9 mmol) were added at room temperature. The mixture was stirred for 15 hours at room temperature. 1N-hydrochloric acid (60 mL, 60 mmol) was added to the reaction liquor, and then methanol was distilled off under reduced pressure. 1N-hydrochloric acid (15 mL, 15 mmol) was added to the obtained aqueous layer, and solids generated therefrom were collected by filtration. The solids were washed with water, and then dried for two days at 50° C. with a vacuum pump, to obtain the title compound (4.41 g, 27.2 mmol, 91%) as a solid.

後処理

  1. distillationmethanol was distilled off under reduced pressure
  2. filtrationgenerated therefrom were collected by filtration
  3. washThe solids were washed with water
  4. customdried for two days at 50° C. with a vacuum pump

出典と根拠

ORDレコード
ord-33b6684450304ffdb882e99925e27393
出典データセット
uspto-grants-2012_03
特許番号
US08129366B2

反応ノート

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