Hydrochloric Acid → Ethyl 7-methoxy-1-benzofuran-2-carboxylate

HRID 636530

반응식

HRID 636530 반응식
[CH2:1]([O:3][C:4]([CH2:6][O:7][C:8]1[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[CH:12][C:9]=1[CH:10]=O)=[O:5])[CH3:2].CC(C)([O-])C.[K+].O.Cl>O1CCCC1>[CH2:1]([O:3][C:4]([C:6]1[O:7][C:8]2[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[CH:12][C:9]=2[CH:10]=1)=[O:5])[CH3:2]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 2229635Ethyl 2-(2-formyl-6-methoxyphenoxy)acetateHCID 23665647Potassium tert-butoxide

생성물 1

HCID 521284Ethyl 7-methoxy-1-benzofuran-2-carboxylate수율 19.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 2-ethoxycarbonylmethoxy-3-methoxybenzaldehyde (2.00 g) and potassium tert-butoxide (96 mg) in tetrahydrofuran (20 ml) was stirred for 1 hour under ice-cooling. Water was added to the reaction mixture, and the solution was neutralized with 1N hydrochloric acid and extracted with ethyl acetate. The extract was washed with water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by preparative thin layer chromatography (n-hexane:ethyl acetate=7:1, v/v) to give 2-ethoxycarbonyl-7-methoxybenzofuran (360 mg).

후처리

  1. temperaturecooling
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with water and brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo
  6. customThe residue was purified by preparative thin layer chromatography (n-hexane

출처 및 근거

ORD 기록
ord-3ee6b20ab77d4a4f953889d5cb4149aa
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06194396B1

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