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Hydrochloric Acid → Ethyl 5-Hydroxy-4-isoxazolecarboxylate

HRID 2080115
ノート
印刷プレビュー

反応式

HRID 2080115 の反応式
[CH2:1]([O:3][C:4](=[O:15])[C:5](=[CH:11]OCC)[C:6]([O:8]CC)=[O:7])[CH3:2].Cl.NO.C([N:21](CC)CC)C.Cl>C(O)C.O>[CH2:1]([O:3][C:4]([C:5]1[C:6](=[O:7])[O:8][NH:21][CH:11]=1)=[O:15])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6871Diethyl (ethoxymethylene)malonateHCID 8471TriethylamineHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 239539Ethyl 5-Hydroxy-4-isoxazolecarboxylate収率 66%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

2-Ethoxymethylene-malonic acid diethyl ester (5.00 g, 23.1 mmol), hydroxylamine hydrochloride (4.01 g, 57.8 mmol) and triethylamine (8.06 mL, 57.8 mmol) were dissolved in ethanol (100 mL), the solution was stirred at room temperature for 17 hours, then, the solution was stirred for 4.5 hours under reflux. The reaction solution was cooled to room temperature, water was added, and 1N hydrochloric acid was added until a salt precipitated. The precipitated salt was collected by filtration, and a hydrochloride salt of the title compound (2.39 g, 15.2 mmol, 66%) was obtained as a white solid.

後処理

  1. stirringthe solution was stirred for 4.5 hours
  2. temperatureunder reflux
  3. temperatureThe reaction solution was cooled to room temperature
  4. customprecipitated
  5. filtrationThe precipitated salt was collected by filtration

出典と根拠

ORDレコード
ord-8f6b96a04688418ea6287645e743fecb
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07932272B2

反応ノート

読み込み中…

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