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Potassium Carbonate → HCID 13321555, Verbindung

HRID 1262817
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1262817
[CH3:1][C:2]1[C:6]([OH:7])=[C:5]([C:8]([O:10][CH:11]([CH3:13])[CH3:12])=[O:9])[S:4][C:3]=1[C:14]([O:16][CH:17]([CH3:19])[CH3:18])=[O:15].O1CCOCC1.C(=O)([O-])[O-].[K+].[K+].[CH2:32]([S:36](Cl)(=[O:38])=[O:37])[CH2:33][CH2:34][CH3:35]>CC(C)=O>[CH3:1][C:2]1[C:6]([O:7][S:36]([CH2:32][CH2:33][CH2:34][CH3:35])(=[O:38])=[O:37])=[C:5]([C:8]([O:10][CH:11]([CH3:13])[CH3:12])=[O:9])[S:4][C:3]=1[C:14]([O:16][CH:17]([CH3:19])[CH3:18])=[O:15]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 11430Potassium CarbonateHCID 312751,4-DioxaneHCID 754301-Butanesulfonyl chlorideHCID 54703303HCID 54703303, Verbindung

Produkt 1

HCID 13321555HCID 13321555, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180Acetone
Lösungsmittel

Versuchsvorschrift

A mixture of 2.3 g (8 mmol) of di-isopropyl 3-methyl-4-hydroxy-2,5-thiophene-dicarboxylate, 30 ml of dioxane, 60 ml of acetone, 1.6 g (120 mmol) of anhydrous potassium carbonate and 1.6 g (10 mmol) of butane-sulfonyl chloride was refluxed for about 10 hours. The mixture was then freed from dioxane and acetone by distillation in vacuo and then added with ethylether, washed with water, and dried with anhydrous magnessium sulfate. The solvent was removed by distillation and then recrystallization was effected from methanol to give 2.8 g (86%) of the desired white crystalline compound. m.p. 59°-61° C.

Aufarbeitung

  1. temperaturewas refluxed for about 10 hours
  2. distillationThe mixture was then freed from dioxane and acetone by distillation in vacuo
  3. additionadded with ethylether
  4. washwashed with water
  5. dry with materialdried with anhydrous magnessium sulfate
  6. customThe solvent was removed by distillation
  7. customrecrystallization
  8. customto give 2.8 g (86%) of the desired white crystalline compound

Quellen und Nachweise

ORD-Eintrag
ord-24cef0660f6249f2a82fb59b0b613559
Quelldatensatz
uspto-grants-1984_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04454131

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