Hydrochloric Acid → 1-Benzofuran-3-carboxylic acid

HRID 1091312노트

반응식

HRID 1091312 반응식
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

참가 물질

6

반응물 4

HCID 313Hydrochloric Acid2회HCID 887MethanolHCID 3939Lithium HydroxideHCID 127770993-Benzofurancarboxylic acid, methyl ester

생성물 1

HCID 5956551-Benzofuran-3-carboxylic acid수율 91.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-33b6684450304ffdb882e99925e27393
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08129366B2

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