Phosphorus sulfide (P2S5) → 2,6-Diphenylthiopyrylium perchlorate

HRID 391496

Reaktionsgleichung

Reaktionsgleichung von HRID 391496
[C:1]1([C:7](=O)[CH2:8][CH2:9][CH2:10][C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:21].[Cl:34]([O-:38])(=[O:37])(=[O:36])=[O:35].[Li+]>C(O)(=O)C>[Cl:34]([O-:38])(=[O:37])(=[O:36])=[O:35].[C:1]1([C:7]2[CH:8]=[CH:9][CH:10]=[C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[S+:21]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

5

Edukt 3

HCID 14817Phosphorus sulfide (P2S5)HCID 804321,3-DibenzoylpropaneHCID 23665649Lithium perchlorate

Produkt 1

HCID 856151432,6-Diphenylthiopyrylium perchlorateAusbeute 24 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

The 1,5-diphenyl-1,5-pentanedione prepared in step 1 (10 mmol, 2.52 g) is mixed with phosphorus pentasulfide (15 mmol, 3.34 g), acetic acid (60 mL) and lithium perchlorate (60 mmol, 6.40 g) in a 100 mL two-necked round-bottomed flask, and then refluxed for 3 hours. The solution then becomes orange and a white precipitate forms. The precipitate is removed by filtration on a sinter funnel and then washed with hot acetic acid. The solution is concentrated on a rotary evaporator and recrystallized by addition of ether (500 mL). The precipitate obtained is filtered off on a sinter funnel and then dried on a rotary evaporator. The product obtained is a yellow solid in a mass of 850 mg. The reaction yield is 24%.

Aufarbeitung

  1. temperaturerefluxed for 3 hours
  2. customThe precipitate is removed by filtration on a sinter funnel
  3. washwashed with hot acetic acid
  4. concentrationThe solution is concentrated on a rotary evaporator
  5. customrecrystallized by addition of ether (500 mL)
  6. customThe precipitate obtained
  7. filtrationis filtered off on a sinter funnel
  8. customdried on a rotary evaporator
  9. customThe product obtained
  10. customThe reaction yield is 24%

Quellen und Nachweise

ORD-Eintrag
ord-acea0814511143e5916fdb418c642130
Quelldatensatz
uspto-grants-2013_02
Patentnummer
US08383931B2

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