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Dimethyl Sulfoxide → HCID 44602516, Verbindung

HRID 448540
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 448540
C(Cl)(=O)C(Cl)=O.CS(C)=O.[Cl:11][CH2:12][CH2:13][C:14]1[C:19](=[O:20])[N:18]2[CH2:21][CH2:22][CH2:23][CH:24]([OH:25])[C:17]2=[N:16][C:15]=1[CH3:26].C(N(CC)CC)C>ClCCl>[Cl:11][CH2:12][CH2:13][C:14]1[C:19](=[O:20])[N:18]2[CH2:21][CH2:22][CH2:23][C:24](=[O:25])[C:17]2=[N:16][C:15]=1[CH3:26]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 155471943-(2-Chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

Produkt 1

HCID 44602516HCID 44602516, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344
Dichloromethane
Lösungsmittel
3×

Versuchsvorschrift

A solution of oxalylchloride (8.8 ml) in dichloromethane (20 ml) was cooled to −65° C. and a solution of dimethyl sulfoxide (6.5 ml) dissolved in dichloromethane (20 ml) was added to it slowly and stirred for 30 min. keeping the temperature at −65° C. a solution of 3-(2-chloroethyl)-9-hydroxy-2-methyl-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidin-4-one (5 grams) (formula-7) dissolved in dichloromethane (30 ml) was added to it very slowly and stirred for 40 min. Triethyl amine was added to the reaction mixture and then quenched with water. The organic layer was separated, washed with aqueous sodium carbonate and water. The solvent from the organic layer was distilled off under reduced pressure to provide the title compound.

Aufarbeitung

  1. additionwas added to it slowly
  2. customat −65° C.
  3. additionwas added to it very slowly
  4. stirringstirred for 40 min
  5. customquenched with water
  6. customThe organic layer was separated
  7. washwashed with aqueous sodium carbonate and water
  8. distillationThe solvent from the organic layer was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-0768b6b37ae74e278e21280929a41dd7
Quelldatensatz
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08481729B2

Notizen zur Reaktion

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