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Methyl iodide → Trifluoroacetic acid

HRID 483903
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HRID 483903 반응식
[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]
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참가 물질

8

반응물 3

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

생성물 3

HCID 6328Methyl iodide수율 14%HCID 6422Trifluoroacetic acid수율 20%HCID 23948Rhodium

시약·촉매·용매 2

HCID 176
Acetic Acid
용매
HCID 962Water용매2회

실험 절차

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.

후처리

  1. additionThe reactor was charged with a solution

출처 및 근거

ORD 기록
ord-fa8540362fb3402a9bcb2261afb3c038
출처 데이터셋
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05227519

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