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ChemicalBook CAS DataBase List Diisobutylcarbinol
108-82-7

Diisobutylcarbinol synthesis

10synthesis methods
By catalytic hydrogenation of diisobutyl ketone
-

Yield:-

Reaction Conditions:

with hydrogen at 60; under 750.075 Torr; for 3 h;

Steps:

2.3. Catalyst testing
General procedure: The hydrogenation of ketones was carried out in the gas phase in flowing H2. The catalysts were tested at 60-100 °C under atmospheric pressure in a Pyrex fixed-bed down-flow reactor (9 mm internal diameter) fitted with an online gas chromatograph (Varian Star 3400 CX instrument with a 30 m × 0.25 mm HP INNOWAXcapillary column and a flame ionisation detector). The temperature in the reactor was controlled by a Eurotherm controller using a thermocouple placed at the top of the catalyst bed. The gas feed contained a variable amount ketone in H2 as a carrier gas. The ketone was fed by passing H2 carrier gas flow controlled by a Brooks mass flow controller through a stainless steel saturator, which held the liquid ketone at appropriate temperature to maintain the chosen reactant partial pressure. The downstream gas lines and valves were heated to 180°C to prevent substrate and product condensation. The gas feed entered the reactor at the top at a flow rate of 20-100 mL min-1. The reactor was packed with 0.2 g catalyst powder of 45-180 m particle size. In some cases, to reduce conversion, a smaller amount of catalyst was used as a homogeneous mixture with silica of a total weight of 0.2 g. Prior to reaction, the catalysts were pretreated in H2 for 1 h at the reaction temperature unless stated otherwise. The dehydration of 2-methyl-4-pentanol was studied similarly, except using N2 as acarrier gas instead of H2. Once reaction started, the downstream gas flow was analysed by the online GC to obtain reactant conversion and product selectivity. The selectivity was defined as moles of product formed per one mole of reactant converted and quoted in mole per cent. The mean absolute percentage error in conversion and selectivity was ≤10% and the carbon balance was maintained within 95%.

References:

Alharbi;Kozhevnikova;Kozhevnikov [Applied Catalysis A: General,2015,vol. 504,p. 457 - 462]

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