StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

HCID 16679760, Verbindung → HCID 16679762, Verbindung

HRID 882316
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 882316
C([NH:4][C@:5]([CH3:15])([C:12]([OH:14])=[O:13])[CH2:6][S:7][C:8]([CH3:11])([CH3:10])[CH3:9])(=O)N>[OH-].[Li+]>[C:8]([S:7][CH2:6][C@@:5]([CH3:15])([C:12]([OH:14])=[O:13])[NH2:4])([CH3:11])([CH3:9])[CH3:10]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 16679760HCID 16679760, Verbindung

Produkt 1

HCID 16679762HCID 16679762, VerbindungAusbeute 80,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3939Lithium HydroxideLösungsmittel

Versuchsvorschrift

N-carbamoyl-S-tert-butyl-α-methyl-L-cysteine (82.4 g, 351.4 mmol) was dissolved in a 18% aqueous lithium hydroxide solution (630 g), and the resultant solution was refluxed in nitrogen for 41 hours. After the solution was allowed to cool down to room temperature, the insoluble substance was filtered off, and the filtrate was adjusted to pH 6 by adding conc. hydrochloric acid (180.1 g). After stirring for about 1 hour, the mixture was cooled to 4° C. to 5° C., and further stirred for 1 hour. The produced crystals were filtered off, washed with water, and then dried under reduced pressure to obtain the title compound as a white solid (53.9 g). As a result of HPLC analysis (column: COSMOSIL 5C18-AR (produced by Nacalai Tesque Inc.), mobile phase: potassium dihydrogen phosphate-phosphoric acid solution (pH 2.0)/acetonitrile=90/10, flow rate: 1.0 ml/min, detection wavelength: 210 nm, column temperature: 40° C.), it was confirmed that the solid was the desired compound (yield 85.7%)

Aufarbeitung

  1. filtrationthe insoluble substance was filtered off
  2. additionby adding conc. hydrochloric acid (180.1 g)
  3. temperaturethe mixture was cooled to 4° C. to 5° C.
  4. stirringfurther stirred for 1 hour
  5. filtrationThe produced crystals were filtered off
  6. washwashed with water
  7. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-3761ecc8d2a847c8be7ab8670644c8ba
Quelldatensatz
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08993800B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion