Hydrochloric Acid → CID 137208342

HRID 1387192

Reaktionsgleichung

Reaktionsgleichung von HRID 1387192
C(OC)(OC)OC.[CH2:8]([C@H:11]([NH2:15])[C:12]([OH:14])=[O:13])[CH2:9][NH2:10].Cl.[C:17](#N)[CH3:18]>CO>[CH3:17][C:18]1[NH:10][CH2:9][CH2:8][C@@H:11]([C:12]([OH:14])=[O:13])[N:15]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 6342AcetonitrileHCID 9005Trimethyl orthoformateHCID 134490L-2,4-Diaminobutyric acid

Produkt 1

HCID 137208342CID 137208342

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

60 ml of trimethyl orthoformate are dissolved in 400 ml of methanol, and reacted with 30 g of L-diaminobutyric acid×2 HCl at 55° C. with constant stirring. After a reaction time of 2 hours, the solvent is evaporated under reduced pressure, the crude product which remains is dissolved in 50 ml of demineralized water, and the solution is neutralized using NaOH. The compound is subsequently purified on an ion retardation column type BIORAD® AG11A8 (Bio-Rad Laboratories GmbH, Munich, Germany) using demineralized water as the eluent, and the product is dried and recrystallized from methanol. The compound obtained can be identified by means of high-pressure liquid chromatography (HPLC), (for example E. Merck, Darmstadt, Germany, LiChroCART® 125-NH2 5μ, eluent: 80% acetonitrile), and is characterized by the following 13C-NMR data:

Aufarbeitung

  1. customAfter a reaction time of 2 hours, the solvent is evaporated under reduced pressure
  2. dissolutionthe crude product which remains is dissolved in 50 ml of demineralized water
  3. customThe compound is subsequently purified on an ion retardation column type BIORAD® AG11A8 (Bio-Rad Laboratories GmbH, Munich, Germany)
  4. customthe product is dried
  5. customrecrystallized from methanol
  6. customThe compound obtained can

Quellen und Nachweise

ORD-Eintrag
ord-4209020922ef4c93b94925e19b8721ac
Quelldatensatz
uspto-grants-2001_07
Patentnummer
US06267973B1

Verknüpfte Notizen

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