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

HRID 636530

反応式

HRID 636530 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 521284Ethyl 7-methoxy-1-benzofuran-2-carboxylate収率 19.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-3ee6b20ab77d4a4f953889d5cb4149aa
出典データセット
uspto-grants-2001_02
特許番号
US06194396B1

関連ノート

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