Tributyl phosphite → Phosphorochloridous acid, dibutyl ester

HRID 437929

Reaktionsgleichung

Reaktionsgleichung von HRID 437929
P(Cl)(Cl)[Cl:2].[CH2:5]([O:9][P:10](OCCCC)[O:11][CH2:12][CH2:13][CH2:14][CH3:15])[CH2:6][CH2:7][CH3:8]>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1>[CH2:5]([O:9][P:10]([Cl:2])[O:11][CH2:12][CH2:13][CH2:14][CH3:15])[CH2:6][CH2:7][CH3:8]

Komponenten

4

Edukt 2

HCID 7623Tributyl phosphiteHCID 24387Phosphorus trichloride

Produkt 1

HCID 4231195Phosphorochloridous acid, dibutyl esterAusbeute 194,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 66133Benzyl triethylammonium chlorideKatalysator

Versuchsvorschrift

17.0 g (0.125 mole) of phosphorus trichloride is added dropwise at 5° to 10° C., with vigorous stirring, to a mixture of 62.5 g (0.25 mole) of tri-n-butylphosphite and 5.0 g of benzyltriethylammonium chloride (water content 7%). After completion of the addition, the reaction mixture is heated to room temperature and stirred for a further 8 hours at this temperature. After separation of the benzyltriethylammonium chloride by filtration there is obtained, by distillation of the filtrate under reduced pressure, 51.8 g (65% of theory, relative to phosphorus trichloride) of di-n-butylchlorophosphite, b.p. 96° to 98° C./10 Torr.

Aufarbeitung

  1. additionAfter completion of the addition
  2. customAfter separation of the benzyltriethylammonium chloride
  3. filtrationby filtration

Quellen und Nachweise

ORD-Eintrag
ord-adf6a42449f34a9ba41391c15c801918
Quelldatensatz
uspto-grants-1977_06
Patentnummer
US04032602

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