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Hydrochloric Acid → HCID 57860414, Verbindung

HRID 1513570
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1513570
[O-]CC.[Na+].[C:5]([O:9][CH2:10][CH3:11])(=[O:8])[CH2:6][SH:7].[Cl:12][C:13]1[C:18]([C:19](OCC)=[O:20])=[C:17](Cl)[C:16]([CH3:25])=[C:15]([CH3:26])[N:14]=1.Cl>C(O)C>[Cl:12][C:13]1[C:18]2[C:19]([OH:20])=[C:6]([C:5]([O:9][CH2:10][CH3:11])=[O:8])[S:7][C:17]=2[C:16]([CH3:25])=[C:15]([CH3:26])[N:14]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 12185Ethyl ThioglycolateHCID 2723922Sodium ethoxideHCID 12749674Ethyl 2,4-dichloro-5,6-dimethylnicotinate

Produkt 1

HCID 57860414HCID 57860414, VerbindungAusbeute 52 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702
Ethanol
Lösungsmittel
2×

Versuchsvorschrift

A 20% solution (1.73 g, 5.08 mmol) of sodium ethoxide in ethanol was diluted with ethanol (5 mL), and ethyl thioglycolate (610 mg, 5.08 mmol) was added. Ethyl 2,4-dichloro-5,6-dimethylpyridine-3-carboxylate (630 mg, 2.54 mmol) was added to the mixture, and the mixture was stirred at room temperature for 18 hr. 2N Hydrochloric acid (3 mL) was added to the reaction mixture and the mixture was partitioned between brine and ethyl acetate. The organic layer was dried over magnesium sulfate and concentrated. The obtained solid was washed with diisopropyl ether-hexane, and dried under reduced pressure to give the title compound (374 mg, 52%) as a white powder.

Aufarbeitung

  1. additionwas added
  2. customthe mixture was partitioned between brine and ethyl acetate
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated
  5. washThe obtained solid was washed with diisopropyl ether-hexane
  6. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-4af7ee5a0640459da2300ab86d8af095
Quelldatensatz
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08217176B2

Notizen zur Reaktion

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