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Hydrochloric Acid → 1-(2,5-Dimethoxy-6-butyl-1,4-benzoquinone-3-yl)-5-[2,5-dimethoxy-6-(2-hydroxyethyl)-1,4-benzoquinon-3-yl]pentane

HRID 1588143
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1588143
[CH3:1][O:2][C:3]1[C:8]([O:9]COC)=[C:7]([CH2:13][CH2:14][CH2:15][CH3:16])[C:6]([O:17][CH3:18])=[C:5]([O:19]COC)[C:4]=1[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][C:28]1[C:33]([O:34]COC)=[C:32]([O:38][CH3:39])[C:31]([CH2:40][CH2:41][O:42]COC)=[C:30]([O:46]COC)[C:29]=1[O:50][CH3:51].Cl.C(=O)([O-])O.[Na+].O=O>O1CCCC1.C(O)(C)C.CO.C1C=CC=CC=1.O1CCCC1.C(O)(C)C>[CH3:1][O:2][C:3]1[C:8](=[O:9])[C:7]([CH2:13][CH2:14][CH2:15][CH3:16])=[C:6]([O:17][CH3:18])[C:5](=[O:19])[C:4]=1[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][C:28]1[C:33](=[O:34])[C:32]([O:38][CH3:39])=[C:31]([CH2:40][CH2:41][OH:42])[C:30](=[O:46])[C:29]=1[O:50][CH3:51]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 4

HCID 313Hydrochloric AcidHCID 977OxygenHCID 516892Sodium BicarbonateHCID 197572401-[2,5-Dimethoxy-4-butyl-3,6-bis(methoxymethoxy)phenyl]-5-[2,5-dimethoxy-3,6-bis(methoxymethoxy)-4-(2-methoxymethyloxyethyl)phenyl]pentane

Produkt 1

HCID 197571941-(2,5-Dimethoxy-6-butyl-1,4-benzoquinone-3-yl)-5-[2,5-dimethoxy-6-(2-hydroxyethyl)-1,4-benzoquinon-3-yl]pentane

Reagenzien, Katalysatoren, Lösungsmittel 5

HCID 241BenzeneLösungsmittelHCID 887MethanolLösungsmittelHCID 3776IsopropanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittelHCID 22597222Tetrahydrofuran 2-propanolLösungsmittel

Versuchsvorschrift

520 Milligrams of 1-[2,5-dimethoxy-4-butyl-3,6-bis(methoxymethoxy)phenyl]-5-[2,5-dimethoxy-3,6-bis(methoxymethoxy)-4-(2-methoxymethyloxyethyl)phenyl]pentane was dissolved in 5 ml of tetrahydrofuran with 5 ml of isopropanol, to this solution was added 1 milliliter of tetrahydrofuran-isopropanol (1:1) solution of 20%-hydrogen chloride, and the whole mixture was stirred at room temperature for 12 hours. After concentrated the reaction mixture, the residue obtained was treated by an azeotrotic distillation with benzene, then dissolved in 8 ml of methanol, further a small amount of sodium hydrogen carbonate was added thereto, and oxygen gas was blown into the solution for 2 hours. This solution was concentrated, and 50 ml of dichloromethane was added to the residue and the solution was washed with water and with a saturated sodium chloride aqueous solution, and concentrated. Then this product was purified by means column chromatography (diameter 2 cm×length 10 cm, adsorbent: "Silica gel 60" manufacture by E. Merck A. G., developing solvent: 30% ethyl acetate-n-hexane) to obtain 231 mg of 1-(2,5-dimethoxy-6-butyl-1,4-benzoquinone-3-yl)-5-[2,5-dimethoxy-6-(2-hydroxyethyl)-1,4-benzoquinon- 3-yl]pentane. Amorphous powdery substance.

Aufarbeitung

  1. concentrationAfter concentrated the reaction mixture
  2. customthe residue obtained
  3. concentrationThis solution was concentrated
  4. addition50 ml of dichloromethane was added to the residue
  5. washthe solution was washed with water and with a saturated sodium chloride aqueous solution
  6. concentrationconcentrated
  7. customThen this product was purified by means column chromatography (diameter 2 cm×length 10 cm, adsorbent

Quellen und Nachweise

ORD-Eintrag
ord-b5534655b5094a698ea01a21826e03f4
Quelldatensatz
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05220042

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