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Ethyl Thioglycolate → HCID 21241315, Verbindung

HRID 1761428
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1761428
[CH3:1][CH2:2][O:3][C:4]([CH2:6][SH:7])=[O:5].[H-].[Na+].Cl[C:11]1[N:16]2[N:17]=[CH:18][N:19]=[C:15]2[N:14]=[C:13]([CH3:20])[CH:12]=1>C(O)C.ClCCl.O>[CH2:2]([O:3][C:4]([CH2:6][S:7][C:11]1[N:16]2[N:17]=[CH:18][N:19]=[C:15]2[N:14]=[C:13]([CH3:20])[CH:12]=1)=[O:5])[CH3:1]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 3

HCID 12185Ethyl ThioglycolateHCID 24758Sodium hydrideHCID 5201277-Chloro-5-methyl-[1,2,4]triazolo[1,5-a]pyrimidine

Produkt 1

HCID 21241315HCID 21241315, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 702EthanolLösungsmittelHCID 962Water
Lösungsmittel
HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

Ethyl thioglycollate, 1.2 g, is dissolved in 30 ml of dry ethanol, to which 400 mg of sodium hydride (60% in an oil) is added under cooling with ice water and stirred for 10 minutes. Then 1.7 g of 7-chloro-5-methyl-[1,2,4]triazolo[1,5-a]pyrimidine and 10 ml of dry dichloromethane are added and stirred for 16 hours. To the reaction mixture, water and dichloromethane are added and the organic layer is separated. The separated organic layer is washed with saline and dried over anhydrous potassium carbonate. The solvent is evaporated under reduced pressure and the residue is purified by column chromatography [on 40 g of silica gel, developed and eluted with ethyl acetate] to give 2.2 g of the desired compound as a colorless powder.

Aufarbeitung

  1. additionis added
  2. stirringstirred for 16 hours
  3. customthe organic layer is separated
  4. washThe separated organic layer is washed with saline
  5. dry with materialdried over anhydrous potassium carbonate
  6. customThe solvent is evaporated under reduced pressure
  7. customthe residue is purified by column chromatography [on 40 g of silica gel, developed and eluted with ethyl acetate]

Quellen und Nachweise

ORD-Eintrag
ord-3715ae08be1442abba4548a5a4379b28
Quelldatensatz
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04826834

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