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Hydrochloric Acid → HCID 21568780, Verbindung

HRID 1579550
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1579550
[C:1]([CH:4]1[CH2:9][CH2:8][CH:7]([CH3:10])[CH2:6][C:5]1=O)(=O)[CH3:2].[CH3:12][CH:13]([C:21]1[CH:22]=[C:23]([OH:28])[CH:24]=[C:25]([CH:27]=1)[OH:26])[CH:14]([CH3:20])[CH2:15][CH2:16][CH2:17][CH2:18][CH3:19].Cl>C(O)(=O)C>[CH3:12][CH:13]([C:21]1[CH:27]=[C:25]([OH:26])[C:24]2[CH:1]([CH3:2])[C:4]3[CH2:9][CH2:8][CH:7]([CH3:10])[CH2:6][C:5]=3[O:28][C:23]=2[CH:22]=1)[CH:14]([CH3:20])[CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 2581765-(3-Methyloctan-2-yl)benzene-1,3-diolHCID 21568772HCID 21568772, Verbindung

Produkt 1

HCID 21568780HCID 21568780, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A solution of 3.6 g. of 2-acetyl-5 -methylcyclohexanone and 5.6 g. of 5-(1,2-dimethylheptyl)resorcinol in 150 ml. of acetic acid is cooled to 15° and saturated with hydrogen chloride gas. The solution is allowed to warm to 25°, stirred for 20 hours and then heated for one hour on a steam bath. The reaction mixture is concentrated in vacuo, water is added and the residue is dissolved in ethyl acetate. The ethyl acetate solution is washed with water, dried (MgSO4) and concentrated to give a residue which is distilled five times, b.p. 195°-200° (0.025 mm.). The distillate is chromatographed on silica gel with benzene as eluant. The second fraction is collected and distilled to give the title compound, b.p. 190°-195° (0.05 mm.).

Aufarbeitung

  1. temperatureto warm to 25°
  2. temperatureheated for one hour on a steam bath
  3. concentrationThe reaction mixture is concentrated in vacuo, water
  4. additionis added
  5. dissolutionthe residue is dissolved in ethyl acetate
  6. washThe ethyl acetate solution is washed with water
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated
  9. customto give a residue which
  10. distillationis distilled five times, b.p. 195°-200° (0.025 mm.)
  11. distillationThe distillate is chromatographed on silica gel with benzene as eluant
  12. customThe second fraction is collected
  13. distillationdistilled

Quellen und Nachweise

ORD-Eintrag
ord-3f065b8bdf1b4489ac934e850355599c
Quelldatensatz
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03931232

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