Glycolic Acid → HCID 178423363, Verbindung

HRID 1244317

Reaktionsgleichung

Reaktionsgleichung von HRID 1244317
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[C:4]([CH3:9])[N:3]=1.[C:10](O)(=O)[CH2:11]O.S(Cl)([Cl:17])=O>C(Cl)(Cl)Cl>[ClH:17].[Cl:17][CH2:11][C:10]1[NH:1][C:2]2=[N:3][C:4]([CH3:9])=[CH:5][CH:6]=[C:7]2[N:8]=1

Komponenten

5

Edukt 3

HCID 757Glycolic AcidHCID 24386Thionyl ChlorideHCID 27344206-Methylpyridine-2,3-diamine

Produkt 1

HCID 178423363HCID 178423363, VerbindungAusbeute 76,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

0.5 g 2,3-Diamino-6-methyl pyridine (4.0 mmol) and 0.37 g glycolic acid were heated at 150° C. for 1 h. The residue was suspended in chloroform (7.0 ml) treated with 1.5 ml thionyl chloride (20 mmol)for 4 h at reflux. The mixture was evaporated and the residue triturated with methanol. After concentration the residue was stirred over night in ether and the suspension was then filtered. The residue on the filter was dried to yield 0.67 g 2-chloromethyl-5-methyl-3H-imidazo[4,5-b]pyridine hydrochloride as a dark brown solid; M.p.: 225–230° C., (dec.).

Aufarbeitung

  1. temperatureat reflux
  2. customThe mixture was evaporated
  3. customthe residue triturated with methanol
  4. concentrationAfter concentration the residue
  5. filtrationthe suspension was then filtered
  6. customThe residue on the filter was dried

Quellen und Nachweise

ORD-Eintrag
ord-30fdcfd2e2b948c78acfda84ab1152c8
Quelldatensatz
uspto-grants-2006_10
Patentnummer
US07122545B2

Verknüpfte Notizen

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