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ChemicalBook CAS DataBase List Cyclohexanecarboxaldehyde
2043-61-0

Cyclohexanecarboxaldehyde synthesis

13synthesis methods
The prepared Grignard reagent was pressed into a dry and clean 20 L reaction bottle, the temperature of the Grignard reagent was cooled to -20° C. and controled at -10±5° C. then 1.506 g of dimethylformamide was dropwise added to the reaction bottle in about 2 h, the temperature of the system was preserved at a temperature below 0° C. for 2 h. 7 L of HCl having a concentration of 4 mol/L was dropwise added to the reaction bottle to terminate the reaction to obtain a reaction product. Suction filtration was performed for the reaction product, an obtained filtrate was standed to enable liquid separation, an obtained water phase was extracted twice with 2.8 L of EA, extracted organic phases were combined and washed with 3 L of saturated salt water, and concentration was performed to obtain 1.608 kg of Cyclohexanecarboxaldehyde having a purity of 96% and a yield of 83%.
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Yield:2043-61-0 99.5%

Reaction Conditions:

with hydrogen in lithium hydroxide monohydrate at 100; under 15001.5 Torr; for 12 h;Autoclave;Green chemistry;

Steps:

Catalytic tests

General procedure: As a typical prodecure, Rh-based catalyst (0.1mol%), olefin (3mmol), and solvent (10mL) were added into a stainless steel autoclave (100mL) with a magnetic stir bar. After sealing and purging with syngas (CO/H2=1:1) for 3 times, the pressure of syngas was adjusted to the desired value and the autoclave was put into a preheated oil bath and stirred with a speed of 1000rpm. After the reaction, the catalysts were taken out from the system by centrifugation and analyzed by gas chromatography equipped with a flame ionization detector and a Supelco γ-DEX 225 capillary column.

References:

Tang, Yongquan;Dong, Ke;Wang, Sai;Sun, Qi;Meng, Xiangju;Xiao, Feng-Shou [Molecular catalysis,2019,vol. 474,art. no. 110408]

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