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Hydrochloric Acid → HCID 22019847, 화합물

HRID 1080913
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HRID 1080913 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

HCID 22019847HCID 22019847, 화합물수율 35%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-94ad8d38b49f4a1c92bd60b1fa6a08d4
출처 데이터셋
uspto-grants-1996_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05583247

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