Palladium Chloride → Palladium

HRID 127175

Reaktionsgleichung

Reaktionsgleichung von HRID 127175
[Pd:1](Cl)Cl.[P:4]([O-:12])([O:9][CH2:10][CH3:11])([O:6][CH2:7][CH3:8])=[O:5]>C(OCC)(=O)C>[Pd:1].[P:4]([O-:12])([O:9][CH2:10][CH3:11])([O:6][CH2:7][CH3:8])=[O:5]

Komponenten

5

Edukt 2

HCID 24290Palladium ChlorideHCID 5166299Diethyl phosphoric acid

Produkt 2

HCID 23938PalladiumHCID 5166299Diethyl phosphoric acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Palladium black is prepared from 13 g of palladium chloride in the manner described in Example 1. A solution of 30.0 g of diethyl phosphate and 2R,3S 3',4',5,7-tetrabenzyloxy-flavan-3-yl phosphate in 1.3 l of ethyl acetate are added. The hydrogenation is carried out for 3 hours and 3.9 l of hydrogen are consumed. The palladium is filtered off and washed twice with 200 ml of ethyl acetate. The combined solutions are evaporated to dryness. 750 ml of water are added to the residue and evaporated under reduced pressure to a volume of approximately 100 ml. This operation is repeated twice then the product is lyophilised. Diethyl phosphate and 2R,3S 3',4',5,7-tetrahydroxy-flavan-3-yl phosphate are obtained. Mp.: 121°-123°.

Aufarbeitung

  1. custom3.9 l of hydrogen are consumed
  2. filtrationThe palladium is filtered off
  3. washwashed twice with 200 ml of ethyl acetate
  4. customThe combined solutions are evaporated to dryness
  5. addition750 ml of water are added to the residue
  6. customevaporated under reduced pressure to a volume of approximately 100 ml

Quellen und Nachweise

ORD-Eintrag
ord-bee01e76c7d6429fbbf53422dd68baa1
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04255336

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