3,4-Bis(diethoxyphosphoryl)-2,3-dihydrothiophene → HCID 59155862, Verbindung

HRID 1662862Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1662862
[CH2:1]([O:3][P:4]([CH:9]1[C:13]([P:14]([O:19][CH2:20][CH3:21])([O:16][CH2:17][CH3:18])=[O:15])=[CH:12][S:11][CH2:10]1)([O:6][CH2:7][CH3:8])=[O:5])[CH3:2]>C1C=CC=CC=1.[O-2].[Mn+4].[O-2]>[CH2:17]([O:16][P:14]([C:13]1[C:9]([P:4]([O:3][CH2:1][CH3:2])([O:6][CH2:7][CH3:8])=[O:5])=[CH:10][S:11][CH:12]=1)([O:19][CH2:20][CH3:21])=[O:15])[CH3:18]

Komponenten

4

Edukt 1

HCID 866384053,4-Bis(diethoxyphosphoryl)-2,3-dihydrothiophene

Produkt 1

HCID 59155862HCID 59155862, VerbindungAusbeute 85,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 241BenzeneLösungsmittelHCID 178418406HCID 178418406, VerbindungLösungsmittel

Versuchsvorschrift

In benzene, 9.740 g (112 mmols) of commercially available manganese (IV) oxide was dissolved, to which 2.010 g (5.60 mmols) of 3,4-bis(diethoxyphosphoryl)-2,3-dihydrothiophene was added at room temperature. Thereafter, the reaction mixture was heated and stirred under reflux for 29 hours. After the reaction, the reaction mixture was cooled down to room temperature and the solid was removed by celite filtration. The filtrate was distilled off under reduced pressure to remove the solvent, and the resulting crude product was purified with a silica gel column (ethyl acetate:methanol=15:1) to obtain the specified substance in the form of a brown solid at a yield of 1.700 g (yield: 85.4%).

Aufarbeitung

  1. additionwas added at room temperature
  2. temperatureThereafter, the reaction mixture was heated
  3. temperatureunder reflux for 29 hours
  4. customAfter the reaction
  5. customthe solid was removed by celite filtration
  6. distillationThe filtrate was distilled off under reduced pressure
  7. customto remove the solvent
  8. customthe resulting crude product was purified with a silica gel column (ethyl acetate:methanol=15:1)
  9. customto obtain the specified substance in the form of a brown solid at a yield of 1.700 g (yield: 85.4%)

Quellen und Nachweise

ORD-Eintrag
ord-46aca065eab84388a9c1436e80c8af96
Quelldatensatz
uspto-grants-2011_10
Patentnummer
US08030438B2

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