Lawesson's reagent → HCID 58423974, Verbindung

HRID 1408563Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1408563
[Br:1][C:2]1[CH:3]=[C:4]2[C:11]3([C:15](=[O:16])[NH:14][C:13](=O)[NH:12]3)[CH2:10][CH:9]([CH:18]3[CH2:23][CH2:22][CH2:21][O:20][CH2:19]3)[O:8][C:5]2=[CH:6][CH:7]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:33])=CC=1>O1CCOCC1>[Br:1][C:2]1[CH:3]=[C:4]2[C:11]3([C:15](=[O:16])[NH:14][C:13](=[S:33])[NH:12]3)[CH2:10][CH:9]([CH:18]3[CH2:23][CH2:22][CH2:21][O:20][CH2:19]3)[O:8][C:5]2=[CH:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 87949Lawesson's reagentHCID 58424192HCID 58424192, Verbindung

Produkt 1

HCID 58423974HCID 58423974, VerbindungAusbeute 40 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A suspension of 6-bromo-2-(tetrahydro-2H-pyran-3-yl)spiro[chroman-4,4′-imidazolidine]-2′,5′-dione (300 mg, 0.79 mmol) and Lawesson's Reagent (319 mg, 0.79 mmol) in dry 1,4-dioxane (4 mL) was heated at 120° C. for 30 minutes in microwave. The mixture was concentrated in vacuo and the residue was purified by preparative TLC to give 6-bromo-2-(tetrahydro-2H-pyran-3-yl)-2′-thioxospiro[chroman-4,4′-imidazolidin]-5′-one (120 mg, 40%).

Aufarbeitung

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue was purified by preparative TLC

Quellen und Nachweise

ORD-Eintrag
ord-d7ecbeee20dc4d9e8b9fa4893d2b45ca
Quelldatensatz
uspto-grants-2014_12
Patentnummer
US08921359B2

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