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Methyl iodide → Trifluoroacetic acid

HRID 483903
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 483903
[Rh:1](I)(I)I.[CH3:5][I:6].[F:7][C:8]([F:13])([F:12])[C:9]([OH:11])=[O:10]>O.C(O)(=O)C>[Rh:1].[CH3:5][I:6].[F:7][C:8]([F:13])([F:12])[C:9]([OH:11])=[O:10]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 3

HCID 6328Methyl iodideHCID 6422Trifluoroacetic acidHCID 4428348Rhodium iodide (RhI3)

Produkt 3

HCID 6328Methyl iodideAusbeute 14 %HCID 6422Trifluoroacetic acidAusbeute 20 %HCID 23948Rhodium

Reagenzien, Katalysatoren, Lösungsmittel

2
HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel2×

Versuchsvorschrift

The reactor was charged with a solution containing rhodium iodide, methyl iodide, water, acetic acid and trifluoroacetic acid (TFAA) in proportions to provide 400 ppm rhodium, 14.0% methyl iodide, 14.0% water and 20.0% TFAA. The reactor was sealed, pressured to approximately 28.14 Kg/cm2 of carbon monoxide partial pressure which was checked at 25° C. The reactor was then slowly vented of its carbon monoxide and then flushed twice with carbon monoxide (7 Kg/cm2). The reactor was then pressureed to 14 Kg/cm2 with carbon monoxide and heated to 120° C. for 2 hours, after which the agitator was turned on to stir at medium speed (100-200 rpm). The reactor was then further heated to 194° C., stirred at high speed (500-600 rpm) and pressured with carbon monoxide to 29 Kg/cm2. The reactor was maintained at a temperature of 194° C. when methanol was fed into the solution and carbon monoxide was introduced continuously at a rate to maintain the pressure in the reactor at about 29 Kg/cm2. The rate of reaction was determined by monitoring the amount of carbon monoxide consumed over a period of time, assuming that the ideal gas law can be applied to carbon monoxide. The rate of CO consumption approximates to the rate of acetic acid production since the formation of by-products is small as shown by products analysis.

Aufarbeitung

  1. additionThe reactor was charged with a solution

Quellen und Nachweise

ORD-Eintrag
ord-fa8540362fb3402a9bcb2261afb3c038
Quelldatensatz
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05227519

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