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

HCID 22850137, Verbindung → 133345-69-4

HRID 2210766
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2210766
[NH2:1][CH2:2][C@H:3]([OH:13])[CH2:4][P:5]([CH3:12])(=[O:11])[O:6]CC(C)C>Cl>[NH2:1][CH2:2][C@H:3]([OH:13])[CH2:4][P:5]([CH3:12])(=[O:6])[OH:11]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 22850137HCID 22850137, Verbindung

Produkt 1

HCID 5310933133345-69-4

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

A solution of 1.1 g of isobutyl P-[3-amino-2(S)-hydroxy-propyl]-P-methyl-phosphinate in 20 ml of 36% aqueous hydrochloric acid is heated to reflux for a period of 12 hours. The reaction mixture is then allowed to cool to room temperature, concentrated under reduced pressure, and co-evaporated four times with 25 ml of water. The crude material is dissolved in water, washed with ether and the aqueous layer is treated with activated charcoal. The solution is filtered hot, the filtrate is concentrated under reduced pressure, the residue dissolved in 20 ml of ethanol and treated with 1 ml of propylene oxide. The mixture is stirred until the precipitated solid is free of halogen. The solid is then filtered and recrystallised from methanol/acetone give P-[3-amino-2(S)-hydroxypropyl]-P- methyl-phosphinic acid, m.p. 221°-222.5°, 31P-NMR spectrum: δ=+38.9 ppm (D2O), [α]D25 =-6.0° (c=0.887% in H2O).

Aufarbeitung

  1. temperatureto reflux for a period of 12 hours
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe crude material is dissolved in water
  4. washwashed with ether
  5. additionthe aqueous layer is treated with activated charcoal
  6. filtrationThe solution is filtered hot
  7. concentrationthe filtrate is concentrated under reduced pressure
  8. dissolutionthe residue dissolved in 20 ml of ethanol
  9. additiontreated with 1 ml of propylene oxide
  10. filtrationThe solid is then filtered
  11. customrecrystallised from methanol/acetone

Quellen und Nachweise

ORD-Eintrag
ord-3986d76505b94334b430cdd882381a4b
Quelldatensatz
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05461040

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion