Epichlorohydrin → HCID 13157038, Verbindung

HRID 964010Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 964010
[CH2:1]([CH:3]1[O:5][CH2:4]1)Cl.[OH:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH:10]=[CH:9][C:8]=1[OH:17].[OH-].[K+]>O>[O:6]1[CH:3]([CH2:4][OH:5])[CH2:1][O:17][C:8]2[CH:9]=[CH:10][C:11]3[C:16]([C:7]1=2)=[CH:15][CH:14]=[CH:13][CH:12]=3

Komponenten

5

Edukt 3

HCID 7835EpichlorohydrinHCID 113181,2-DihydroxynaphthaleneHCID 14797Potassium Hydroxide

Produkt 1

HCID 13157038HCID 13157038, VerbindungAusbeute 74,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

Epichlorohydrin (2.32 g) was added dropwise to a stirred solution of 1,2-dihydroxynaphthalene (4.0 g) and potassium hydroxide (4.0 g) in water (32 ml) and the resulting mixture stirred at 60°-80° C. for 2.5 hours then poured into water (100 ml). The product was extracted into ether (6×100 ml), a small volume of methanol being added to aid solubility. The combined extracts were washed with aqueous sodium hydroxide solution (1M), then water, and dried over magnesium sulphate. The solvent was removed in vacuo to give crude 1-(naphtho[1,2-b]dioxan-2-yl)methanol (4.0 g) as a dark oil which was used without further purification.

Aufarbeitung

  1. extractionThe product was extracted into ether (6×100 ml)
  2. additiona small volume of methanol being added
  3. washThe combined extracts were washed with aqueous sodium hydroxide solution (1M)
  4. dry with materialwater, and dried over magnesium sulphate
  5. customThe solvent was removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-bf249c08c4b249578a1c3b95f839accf
Quelldatensatz
uspto-grants-1998_06
Patentnummer
US05767116

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