2-Fluoro-4-cyanobenzyl bromide synthesis
- Product Name:2-Fluoro-4-cyanobenzyl bromide
- CAS Number:105942-09-4
- Molecular formula:C8H5BrFN
- Molecular Weight:214.03
170572-49-3
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105942-09-4
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Yield:105942-09-4 94%
Reaction Conditions:
with NBS;2,2'-azobisisobutyronitrile in 1,2-dichloro-ethane at 75;Large scale;Reagent/catalyst;Temperature;Solvent;
Steps:
1; 2.1; 3.1; 4.1; 5.1 The first step:
550 g (1 eq) of 3-fluoro-4-methylbenzonitrile, 50 g (0.074 eq) of azobisisobutyronitrile and 1 kg of dichloroethane were added to the storage tank A. The solution was stirred, and 797 g (1.1 eq) of N-bromosuccinimide and 1.75 kg of dichloroethane were added to storage tank B. The microreactor 1 was heated to 75°C, and the solution in the storage tank A was sent to the first plate of the microreactor 1 through the pump A at a flow rate of 16 g/min; the solution in the storage tank B was passed through the slurry pump B at a flow rate of 25.5 g/min. It was sent to the first plate of microreactor 1; mixed reaction, after the bromination reaction of 6 plates, the color of the solution changed from light yellow to colorless, sampling GC detection, the reaction of raw materials was completed, product: dibromide = 98:2, The temperature was controlled at 20 to 35°C, and the reaction was dropped into 4 kg of water for quenching under stirring; post-processing: layering, the organic layer was washed once with 2 kg of water, The organic layer was concentrated to obtain 819.7 g of a light yellow solid product of 4-bromomethyl-3-fluorobenzonitrile, GC: 97.2%, and the isolated yield was 94%.
References:
CN113816874,2021,A Location in patent:Paragraph 0015; 0036-0041; 0043-0045; 0047-0049; 0051-0053
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