Phosphorus sulfide (P2S5) → 1-Methyl-5-Methoxy-2-Indolinethione

HRID 1086511Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1086511
C(=O)(O)[O-].[Na+].[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[C:14](=[CH:15][CH:16]=1)[N:13]([CH3:17])[C:12](=O)[CH2:11]2.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:20]>O1CCCC1>[CH3:17][N:13]1[C:14]2[C:10](=[CH:9][C:8]([O:7][CH3:6])=[CH:16][CH:15]=2)[CH2:11][C:12]1=[S:20]

Komponenten

5

Edukt 3

HCID 14817Phosphorus sulfide (P2S5)HCID 516892Sodium BicarbonateHCID 91021941,3-Dihydro-5-methoxy-1-methyl-2H-indol-2-one

Produkt 1

HCID 137767581-Methyl-5-Methoxy-2-Indolinethione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

18.5 g (0.22 mol) of sodium bicarbonate are added to a solution of 19.5 g (0.11 mol) of 5-methoxy-1-methyl-2-indolinone prepared according to A. H. BECKETT, R. W. DAISLEY and J. WALKER (Tetrahedron 1968, 24 6093) and 16.5 g (0.037 mol) of phosphorus pentasulfide in 200 ml of tetrahydrofuran. The reaction medium is heated to a temperature of 50° C. for 1 h 30 min and then filtered and concentrated on a water bath under vacuum. The residue is taken up with ice-cold water and the mixture is extracted with methylene chloride. The organic phase is washed with saturated sodium chloride solution, dried and evaporated. The residue is used in the next stage without further treatment.

Aufarbeitung

  1. customprepared
  2. filtrationfiltered
  3. concentrationconcentrated on a water bath under vacuum
  4. extractionthe mixture is extracted with methylene chloride
  5. washThe organic phase is washed with saturated sodium chloride solution
  6. customdried
  7. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-5b94579deea04c9a84ebb9428ed474c1
Quelldatensatz
uspto-grants-1991_07
Patentnummer
US05030646

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