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Methyl iodide → Trifluoroacetic acid

HRID 483903
ノート
印刷プレビュー

反応式

HRID 483903 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

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

生成物 3

HCID 6328Methyl iodide収率 14%HCID 6422Trifluoroacetic acid収率 20%HCID 23948Rhodium

試薬・触媒・溶媒 2

HCID 176
Acetic Acid
溶媒
HCID 962Water溶媒2 回

実験手順

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.

後処理

  1. additionThe reactor was charged with a solution

出典と根拠

ORDレコード
ord-fa8540362fb3402a9bcb2261afb3c038
出典データセット
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05227519

反応ノート

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