ChemicalBook CAS DataBase List Pentafluorobenzaldehyde

Pentafluorobenzaldehyde synthesis

12synthesis methods

Product Name:Pentafluorobenzaldehyde
CAS Number:653-37-2
Molecular formula:C7HF5O
Molecular Weight:196.07

Pentafluorobenzaldehyde is prepared by the reaction ofpentafluorophenylmagnesium bromide, iodide or chloride, or of pentafluorophenyllithium with ethyl-ortho-formiate or 3,4-dihydro-6-methyl-3-(para-tolyl)-quinazoline methiodide. Higher yields of pentafluorobenza1dehyde have been obtained by the reaction with N-methy1formanilide. Pentafluorobenzaldehyde may be prepared also by the reaction of pentafluorobenzonitrile with anhydrous SnClz in ethereal solution of HCl with subsequent hydrolsis of the intermediate (62% yield).

773-82-0 Synthesis

773-82-0
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$7.00/5g

653-37-2
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$6.00/1g

Yield:653-37-2 61.5%

Reaction Conditions:

with formic acid;nickel-aluminum alloy in water at 65; for 1 h;Inert atmosphere;Large scale;Green chemistry;

Steps:

1

to the condenser, Mechanical agitation, thermometer casing 50L The reactor was charged with pentafluorobenzonitrile 4.9 kg, Formic acid 15Kg, water 8.5Kg, access to nitrogen protection, Heating up to 65 ° C, The nickel-aluminum alloy powder 2.2Kg into eight batches into the reactor, The process of exothermic, maintained in the reflow state. After the addition of the nickel-aluminum alloy powder, the mixture was refluxed for 1 hour, Sampling, Gas Phase Detection of Pentafluorobenzonitrile 0.2%, cool to room temperature, filter, The filtrate was extracted with 25 Kg of water and 10 Kg of dichloromethane, Separate the water layer and add it 10Kg dichloromethane extraction time, After the organic layers were extracted twice, A 5% aqueous solution of sodium hydrogencarbonate was added, Adjust the pH to 6 ~ 7, separated from the reservoir, Distillation at atmospheric pressure to recover dichloromethane, Distillation of the mother liquor after distillation, In the pressure -0.09Mpa, Top temperature 108 ° C steamed product pentafluorobenzaldehyde 3. lKg (Receiving tube need to heat, easy to solidify the product after blocking) Melting point 24 ~ 28 ° C, Content of 98.7%, Yield 61.5%.

References:

CN106397149,2017,A Location in patent:Paragraph 0225-0226

440-60-8 Synthesis