Phosphinic Acid → Bis(3,4-dimethoxyphenyl)ditelluride

HRID 543065Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 543065
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([Te:11](Cl)(Cl)Cl)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[PH2](O)=O>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([Te:11][Te:11][C:5]2[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

Komponenten

4

Edukt 2

HCID 4124402Phosphinic AcidHCID 124943393,4-Dimethoxyphenyltellurium trichloride

Produkt 1

HCID 4345922Bis(3,4-dimethoxyphenyl)ditelluride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

3,4-Dimethoxyphenyltellurium trichloride (37.2 g=0.1 mole) was dissolved in absolute ethanol (500 ml), and the slightly turbid solution was filtered. To the rapidly stirred solution was added, at room temperature, 50% aqueous hypophosphorous acid (30 ml, ≃0.3 mole) as rapidly as possible. There was a brief appearance of a brown solution color, before the entire solution set to a mass of black fibrous crystals. The product was collected after 15 minutes by filtration using rubber dam to compact the highly solvated crystal mass. The product was washed with water and then air dried to yield 25.2 g, 95% of theory, black fibrous crystals, m.p. 134°-136° C. Recrystallization from isopropanol raised the m.p. to 136°-139° C. C, H and Te elemental analyses were in agreement with the structural formula.

Aufarbeitung

  1. filtrationthe slightly turbid solution was filtered
  2. additionTo the rapidly stirred solution was added, at room temperature
  3. filtrationThe product was collected after 15 minutes by filtration
  4. washThe product was washed with water
  5. customair dried
  6. customto yield 25.2 g, 95% of theory, black fibrous crystals, m.p. 134°-136° C
  7. customRecrystallization from isopropanol
  8. temperatureraised the m.p. to 136°-139° C

Quellen und Nachweise

ORD-Eintrag
ord-437a0c1648904372956c2201c28c761b
Quelldatensatz
uspto-grants-1987_04
Patentnummer
US04661438

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