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Hydrochloric Acid → HCID 22019847、化合物

HRID 1080913
ノート
印刷プレビュー

反応式

HRID 1080913 の反応式
[C:1]([C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([C:12]([CH2:15][CH3:16])([CH3:14])[CH3:13])[C:7]=1[OH:17])([CH2:4][CH3:5])([CH3:3])[CH3:2].[C:18]([OH:22])(=[O:21])[CH:19]=O.Cl>C(O)(=O)C>[C:12]([C:8]1[C:7](=[O:17])[C:6]([C:1]([CH2:4][CH3:5])([CH3:3])[CH3:2])=[CH:11][C:10](=[CH:19][C:18]([OH:22])=[O:21])[CH:9]=1)([CH2:15][CH3:16])([CH3:14])[CH3:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 760Glyoxylic AcidHCID 144965062,6-Di-tert-pentylphenol

生成物 1

HCID 22019847HCID 22019847、化合物収率 35%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

15.0 g (0.064 Mol) of 2,6-di-tert-amylphenol and 11.4 g (0.077 mol) of 50% aqueous glyoxylic acid are dissolved in 100 ml of acetic acid. The solution is then saturated at 15°-25° C. with hydrogen chloride gas and stirred at room temperature for additional four hours. The mixture is then poured in 400 ml of ice-water and extracted with 200 ml of ethyl acetate. The ethyl acetate layer is washed several times with water, dryed over anhydrous sodium sulfate, and evaporated in vacuo. The oily residue is then chromatographed on silica gel with ethyl acetate:hexane (1:20→1:3). The pure fractions are recrystallized from hexane to give 6.5 g of the title compound as orange needles, melting at 109°-110° C.

後処理

  1. extractionextracted with 200 ml of ethyl acetate
  2. washThe ethyl acetate layer is washed several times with water
  3. customevaporated in vacuo
  4. customThe oily residue is then chromatographed on silica gel with ethyl acetate:hexane (1:20→1:3)
  5. customThe pure fractions are recrystallized from hexane

出典と根拠

ORDレコード
ord-94ad8d38b49f4a1c92bd60b1fa6a08d4
出典データセット
uspto-grants-1996_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05583247

反応ノート

読み込み中…

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