3-Fluorobenzyl alcohol synthesis
- Product Name:3-Fluorobenzyl alcohol
- CAS Number:456-47-3
- Molecular formula:C7H7FO
- Molecular Weight:126.13
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456-47-3
GENERAL STEPS: Prior to use, 0.05 g of 5 wt% Pt/C catalyst was pretreated in a stream of hydrogen at 673 K for 2 hours. Subsequently, the pretreated catalyst was mixed with 20 mL of solvent (e.g., ethanol) and the mixture was transferred to a 100 mL high-pressure reactor. After filling the reactor with hydrogen at 4.0 MPa, the reaction was initiated and hydrogenation was carried out at a set temperature. The reaction was terminated after reaching a predetermined time, and the products were analyzed by a gas chromatograph (GC-2014, Shimadzu Co.) equipped with a capillary column (DM-WAX, 30 m × 0.32 mm × 0.25 μm) coupled with a flame ionization detector (FID).
352-70-5
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455-38-9
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456-47-3
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456-48-4
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Yield:-
Reaction Conditions:
Stage #1:m-Fluorotoluene with 5,10,15,20-tetrakis(4-methylphenyl)porphyrinatocopper(II);C40H32MnN8;cobalt(II) diacetate tetrahydrate at 186; under 13501.4 Torr;
Stage #2: with water at 145; under 9000.9 Torr;
Steps:
14
Adding a time of the oxidation reactor fresh fluorine catalyst is dissolved in the toluene Co(Ac)2·4H2O, having the general formula (IV) of a metal phthalocyanine structure (R1=CH3CH2, R2=H, M=Mn), having the general formula (I) structural metal porphyrin (R1=R2=H, R3=CH3, M=Cu) mixture, the total concentration of 380 ppm. When the device was operated at steady state, the flow rate of fresh m-fluorotoluene in the oxidation reactor was 15.7 mL / h. The mean residence time of the oxidation reactor in liquid phase was 2.8 h, The air was continuously fed into the oxidation reactor to maintain the reaction temperature of 186 °C and the reaction pressure of 1.8 MPa. The volume of water added to the hydrolysis reactor was 0.24: 1 with the oxidation reaction liquid entering the hydrolysis reactor, and the pressurized air was continuously fed to maintain a reaction temperature of 145 °C and a reaction pressure of 1 in the hydrolysis reactor. 2MPa. The residence time of the liquid phase in the hydrolysis reactor is 3.2h. The liquid phase at the outlet of the hydrolysis reactor was continuously fed into a liquid-liquid delaminator at a temperature of 109 ° C and a pressure of 1.1MPa. The conversion of m-fluorotoluene in the system was 95.8% after sampling and analysis, The selectivity of m-fluorobenzyl alcohol, m-fluorobenzaldehyde and m-fluorobenzoic acid were 43.1%, 51.8% and 5.1%, respectively. Other byproducts were not detected.
References:
Quzhou Qunying Chemical Technology Co. Ltd.,;Wang, Qinbo;Xiong, Zhenhua;Chen, Chuxiong CN105237317, 2016, A Location in patent:Paragraph 0085; 0086
456-48-4
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456-47-3
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456-47-3
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