Water → HCID 178493400, Verbindung

HRID 441052

Reaktionsgleichung

Reaktionsgleichung von HRID 441052
[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([O:10][CH3:11])[C:3]=1[C:12](=[O:14])[CH3:13].[C:15](=[S:17])=S.O.S(=O)(=O)(O)O>C1(C)C=CC=CC=1>[OH:14][C:12]1[C:3]2[C:2](=[CH:7][C:6]([O:8][CH3:9])=[CH:5][C:4]=2[O:10][CH3:11])[O:1][C:15](=[S:17])[CH:13]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 6348Carbon DisulfideHCID 66654Xanthoxylin

Produkt 1

HCID 178493400HCID 178493400, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel4×

Versuchsvorschrift

336.0 g of potassium t-butoxy was suspended in 2 liters of toluene. Under cooling on ice, 2 liters of 196.0 g of 2'-hyroxy-4',6'-dimethoxyacetophenone and 72.0 ml carbon disulfide in toluene were added dropwise to said suspension. The mixture was stirred for 20 hours at room temperature, and 7 liters of water was added for extraction of a toluene layer. This toluene solution was adjusted to pH 4-5 by addition of 800 ml of 10% sulfuric acid (aq.) and was then stirred for 5 hours at room temperature. The solution was allowed to stand overnight. The resulting yellow crystals were collected by filtration under reduced pressure, sufficiently washed with water and dried at 50° C. for 3 days under reduced pressure, thus giving rise to 160.0 g crude 4-hydroxy-5,7-dimethoxychromene-2-thion.

Aufarbeitung

  1. additionwere added dropwise
  2. stirringwas then stirred for 5 hours at room temperature
  3. waitto stand overnight
  4. filtrationThe resulting yellow crystals were collected by filtration under reduced pressure
  5. washsufficiently washed with water
  6. customdried at 50° C. for 3 days under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-387f65fb15364149b6a36464951de885
Quelldatensatz
uspto-grants-1996_05
Patentnummer
US05521216

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