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Hydrochloric Acid → HCID 19863826, 화합물

HRID 1165100
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HRID 1165100 반응식
[CH3:1][C:2]([CH2:13][CH2:14][CH2:15][CH:16]([CH3:28])[CH2:17][CH2:18][CH2:19][CH:20]([CH3:27])[CH2:21][CH2:22][CH2:23][CH:24]([CH3:26])[CH3:25])=[CH:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][C:6]=1[OH:12].Cl.O>CO>[CH3:1][C:2]1([CH2:13][CH2:14][CH2:15][CH:16]([CH3:28])[CH2:17][CH2:18][CH2:19][CH:20]([CH3:27])[CH2:21][CH2:22][CH2:23][CH:24]([CH3:26])[CH3:25])[CH2:3][CH2:4][C:5]2[C:6](=[CH:7][C:8]([OH:11])=[CH:9][CH:10]=2)[O:12]1
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 54539569HCID 54539569, 화합물

생성물 1

HCID 19863826HCID 19863826, 화합물수율 70%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 4-(3,7,11,15-tetramethyl-2-hexadecenyl)-1,3-benzenediol (870 mg; 2.24 mmole) and conc. hydrochloric acid (2.0 ml) in methanol (15 ml) was heated under reflux for 4 hours, then the reaction solution was poured into 70 ml of water and was extracted twice with isopropyl ether (50 ml). The extract was washed with 100 ml of water (twice) and 100 ml of saturated aqueous solution of sodium chloride (once), followed by drying it over anhydrous magnesium sulfate, distilling off the solvent and subjecting the resultant residue to silica gel column chromatography to thus obtain 610 mg of the title compound from the fractions eluted with hexane-ethyl acetate (10:1). Yield=70%.

후처리

  1. temperatureunder reflux for 4 hours
  2. extractionwas extracted twice with isopropyl ether (50 ml)
  3. washThe extract was washed with 100 ml of water (twice) and 100 ml of saturated aqueous solution of sodium chloride (once),
  4. dry with materialby drying it over anhydrous magnesium sulfate
  5. distillationdistilling off the solvent
  6. washeluted with hexane-ethyl acetate (10:1)

출처 및 근거

ORD 기록
ord-4e1465766be14dd39a17097936b2bc2f
출처 데이터셋
uspto-grants-1990_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04906669

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