3,4-Difluorobenzaldehyde

Light Yellow Clear Liquid

5L four-necked flask, mechanical stirring, nitrogen protection, followed by adding magnesium strips, 400g iodine granules in tetrahydrofuran, further, 41.7 g of 2-chloropropane was added at room temperature, 10min after the addition, temperature up to 40 deg. C, cooling, 30-40 ° C drop with a solution of 2-chloropropane, 4.5h dropwise additon is completed, insulation 1h, basically no magnesium. Cooling, a solution of 3, 4-difluorobromobenzene (654 g of 3, 4-difluorobromobenzene in 700 g of tetrahydrofuran) was dropwise added at 0 to 10 ° C, and the addition was completed in 50 minutes. Insulation reaction, can be done at room temperature. Reaction is completed, cooling, a solution of DMF (291.3 g of DMF in 300 g of tetrahydrofuran) was added dropwise at 0-10 ° C over 40 min. The temperature below 10 deg. C, dropping 700g of water, and then dropping concentrated hydrochloric acid to adjust pH to about 4, about 840g hydrochloric acid, phase separation, the lower aqueous phase with 500g toluene extraction twice, combine the organic layer, washed once with 500 g of saturated saline solution, and washed once with 500 g of water. 65 deg. C pump vacuum concentration to no solvent, was crude, vacuum distillation, the purity of more than 99.5percent, 86percent yield.6.06 g of cobalt acetate and 6.06 g of sodium molybdate were dissolved in 200 ml3, 4-difluorotoluene and 200 mlAcetic acid to form a mixed solution, At this time η (cobalt acetate):Η (3, 4-difluorotoluene) = 0.015:1, 6.06 g of sodium bromide was dissolved in 15percentH202formH202- acetic acid solution, At this time η (sodium bromide):Η (3, 4-difluorotoluene) = 0.015: 1, 3, 4-difluorotoluene-acetic acid solutionWith H22-acetic acid solution at 8.33 ml / min and 16.67 ml / min, respectivelyOf the flow rate through the constant flow into the continuous heat exchanger tube reactor, At this time η (H2 2): η (3, 4-difluoromethyl = 2: 1, The reaction temperature was controlled Using Figure 2 microchannel reactor, Control the reaction temperature65 ° C, residence time 200s. Export material 0 ° C cooling, The reaction was quenched with difluoromethane.After GC analysis, The conversion of 3, 4-difluorotoluene was 42.0percent and the yield of 3, 4-difluorobenzaldehyde was 30.7percent.

Metabolic

Molecular Weight:142.10
XLogP3:1.8
Hydrogen Bond Acceptor Count:3
Rotatable Bond Count:1
Exact Mass:142.02302107
Monoisotopic Mass:142.02302107
Topological Polar Surface Area:17.1
Heavy Atom Count:10
Complexity:127
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes