Acetic Acid → HCID 13345321, Verbindung

HRID 1254079Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1254079
[CH3:1][C:2]1[N:7](C(O)=O)[CH:6]([C:11]([OH:13])=[O:12])[CH:5]=[CH:4][CH:3]=1.[C:14](O)(=[O:16])C.N1C=CC=CC=1.CCCCCC>COCCOC.CCOCC>[CH3:1][C:2]1[N:7]=[C:6]2[C:11](=[O:12])[O:13][C:14](=[O:16])[C:5]2=[CH:4][CH:3]=1

Komponenten

7

Edukt 4

HCID 176Acetic AcidHCID 1049PyridineHCID 8058HexaneHCID 67315455HCID 67315455, Verbindung

Produkt 1

HCID 13345321HCID 13345321, VerbindungAusbeute 74,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 80711,2-DimethoxyethaneLösungsmittel

Versuchsvorschrift

A solution of 6-methyl-1,2-pyridine dicarboxylic acid (25 g, 138 mmol) and acetic acid (42 mL, 733 mmol) in DME (150 mL) is treated with pyridine (22 mL, 272 mmol) and stirred at room temperature for 2 h. The pale yellow solution is diluted with ether (250 mL) and then hexane (1250 mL) is added slowly. A white precipitate is formed. The solution is cooled to 0° C. for 30 min and the white solid is collected by filtration. The solid is washed with hexane and dried to give the title compound as a white solid (16.7 g, 74%).

Aufarbeitung

  1. customA white precipitate is formed
  2. temperatureThe solution is cooled to 0° C. for 30 min
  3. filtrationthe white solid is collected by filtration
  4. washThe solid is washed with hexane
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-509f1e350f9b44b19cf6b6ee8929bcde
Quelldatensatz
uspto-grants-2013_06
Patentnummer
US08455535B2

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