Lawesson's reagent → HCID 5324342, Verbindung

HRID 1099097

Reaktionsgleichung

Reaktionsgleichung von HRID 1099097
COC1C=CC(P2(=S)SP(C3C=CC(OC)=CC=3)(=S)[S:10]2)=CC=1.[C:23]([O:27][C:28](=[O:35])[NH:29][C@H:30]([CH3:34])[C:31]([NH2:33])=O)([CH3:26])([CH3:25])[CH3:24]>COCCOC>[C:23]([O:27][C:28](=[O:35])[NH:29][C@H:30]([CH3:34])[C:31]([NH2:33])=[S:10])([CH3:26])([CH3:25])[CH3:24]

Komponenten

4

Edukt 2

HCID 87949Lawesson's reagentHCID 7015296Boc-D-Ala-NH2

Produkt 1

HCID 5324342HCID 5324342, VerbindungAusbeute 203,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 80711,2-DimethoxyethaneLösungsmittel

Versuchsvorschrift

2,4-Bis(4-methoxyphenyl)-2,4-dithioxo-1,3,2,4-dithiadiphosphetane (1.6 g, 0.0038 mol) was added to a solution of tert-butyl[(1R)-2-amino-1-methyl-2-oxoethyl]carbamate (1.45 g, 0.00770 mol) in 1,2-dimethoxyethane (40 mL). The resulting suspension was stirred at RT for 5 h. After removal of solvent the residue was taken up into ethyl acetate. It was washed with 0.1 N NaOH solution, water, brine; dried over Na2SO4. After filtration the filtrate was concentrated to yield 1.58 g of the product. (yield: ˜100%).

Aufarbeitung

  1. customAfter removal of solvent the residue
  2. washIt was washed with 0.1 N NaOH solution, water, brine
  3. dry with materialdried over Na2SO4
  4. filtrationAfter filtration the filtrate
  5. concentrationwas concentrated

Quellen und Nachweise

ORD-Eintrag
ord-2367931cdfd842fa98bc713e4691fa14
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08143251B2

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