Potassium Bromide → HCID 54402307, Verbindung

HRID 1460439

Reaktionsgleichung

Reaktionsgleichung von HRID 1460439
N[C@@H:2]([C:7]([OH:9])=[O:8])[CH2:3][C:4](=[O:6])[NH2:5].[K+].[Br-:11].N([O-])=O.[Na+]>OS(O)(=O)=O.O>[Br:11][C@H:2]([CH2:3][C:4](=[O:6])[NH2:5])[C:7]([OH:9])=[O:8]

Komponenten

6

Edukt 3

HCID 253877Potassium BromideHCID 439600D-AsparagineHCID 23668193Sodium Nitrite

Produkt 1

HCID 54402307HCID 54402307, VerbindungAusbeute 78,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

D-Asparagine 1 (195.0 g, 1.299 mol) and KBr (461 g, 3.87 mol) were dissolved in 3M H2SO4 (1720 ml). The solution was cooled in an ice-MeOH bath and stirred while a solution of NaNO2 (111.5 g. 1.62 mol) in H2O (200 ml) was added dropwise over 85 minutes. The temperature of the reaction mixture was kept at -5° during the addition and for an additional 60 minutes. The white precipitate was collected, washed twice with ice-cold water, and dried i.v. to give the bromo derivative 2 (198.9 g, 78%): [α]D +69.0° (C., 4.63, EtOH). ##STR82##

Aufarbeitung

  1. temperatureThe solution was cooled in an ice-MeOH bath
  2. additionwas added dropwise over 85 minutes
  3. additionThe temperature of the reaction mixture was kept at -5° during the addition and for an additional 60 minutes
  4. customThe white precipitate was collected
  5. washwashed twice with ice-cold water
  6. customdried i.v

Quellen und Nachweise

ORD-Eintrag
ord-9a280d18b3fb436da62447f28a3fde52
Quelldatensatz
uspto-grants-1991_12
Patentnummer
US05071843

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