Water → HCID 33240185, Verbindung

HRID 1027478Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1027478
C(N(CC)CC)C.Cl.[CH2:9]([O:11][C:12](=[O:20])[CH:13]([NH2:19])[C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH3:10].[F:21][C:22]1[CH:23]=[C:24]([CH:28]=[CH:29][CH:30]=1)[C:25](Cl)=[O:26].O>ClCCl>[CH2:17]([O:16][C:14](=[O:15])[CH:13]([NH:19][C:25](=[O:26])[C:24]1[CH:28]=[CH:29][CH:30]=[C:22]([F:21])[CH:23]=1)[C:12]([O:11][CH2:9][CH3:10])=[O:20])[CH3:18]

Komponenten

6

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 743763-Fluorobenzoyl chlorideHCID 3084143Propanedioic acid, 2-amino-, 1,3-diethyl ester, hydrochloride (1:1)

Produkt 1

HCID 33240185HCID 33240185, VerbindungAusbeute 94,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

36.1 ml of triethylamine were added to a solution of 25 g of aminomalonic acid diethyl ester hydrochloride in 200 ml of dichloromethane with cooling in an ice bath. Then a solution of 18.7 g of 3-fluoro-benzoyl chloride in 100 ml of dichloromethane was added dropwise. After stirring for 2 h at 0° C., 100 ml of water were added dropwise. The layers were separated, and the aqueous layer was extracted with 100 ml of dichloromethane. The combined organic layers were dried with magnesium sulfate, filtered and evaporated to give 33.2 g of the crude title compound.

Aufarbeitung

  1. temperaturewith cooling in an ice bath
  2. customThe layers were separated
  3. extractionthe aqueous layer was extracted with 100 ml of dichloromethane
  4. dry with materialThe combined organic layers were dried with magnesium sulfate
  5. filtrationfiltered
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-ebf9bae0f01946c8878fe652c69c9b5e
Quelldatensatz
uspto-grants-2014_05
Patentnummer
US08735387B2

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