Category: 14160-91-9

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 14160-91-9, name is 4,6-Dichloro-2-methylpyrimidine-5-carbaldehyde. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 14160-91-9

To a stirred solution of A-1a (150.00 g, 785.28 mmol, 1.0 equiv.) in benzene (1500 mL) ethylene glycol (48.69 g, 785.28 mmol, 1.0 equiv.) and a catalytic amount of p-toluenesulphonic acid (13.51 g, 78.53 mmol, 0.1 equiv.) are added. The reaction mixture is refluxed until full conversion of the starting material is observed. The solvent is evaporated under reduced pressure, the residue diluted with DCM and washed with an aqueous sodiumbicarbonate solution. Organic layers are combined, dried (Na 2SO 4) and concentrated under reduced pressure. Further purification by flash column chromatography (eluent: 10% ethyl acetate in hexane) yields the desired product A-2a.

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Reference:
Patent; Boehringer Ingelheim International GmbH; RAMHARTER, Juergen; KOFINK, Christiane; STADTMUELLER, Heinz; WUNBERG, Tobias; HOFMANN, Marco Hans; BAUM, Anke; GMACHL, Michael; RUDOLPH, Dorothea Ingrid; SAVARESE, Fabio; OSTERMEIER, Markus; FRANK, Markus; GILLE, Annika; GOEPPER, Stefan; SANTAGOSTINO, Marco; WIPPICH, Julian; (175 pag.)US2019/194192; (2019); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Reference of 14160-91-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 14160-91-9, name is 4,6-Dichloro-2-methylpyrimidine-5-carbaldehyde, molecular formula is C6H4Cl2N2O, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Intermediate 44: 4,6-Dichloro-2-methylpyrimidine-5-carbonyl chloride Sulfuryl chloride (0.114 mL, 1.42 mmol) and 2,2′-azobisisobutyronitrile (6.88 mg, 0.04 mmol) were added to a solution of 4,6-dichloro-2-methylpyrimidine-5-carbaldehyde (Intermediate 45; 0.16 g, 0.84 mmol) in CC14 (3 mL). The reaction was heated at reflux for 3 hours then cooled. The rm was injected directly onto a column. The crude product was purified by flash silica chromatography, eluting with DCM. Pure fractions were evaporated to dryness to afford the title compound (0.180 g, 95 %) as a colourless oil. 1H NMR (400 MHz, CDC13) delta 2.77 (3H, s). m/z (ES+) M-COC1-H = 161

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Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; BIRCH, Alan, Martin; GOLDBERG, Frederick, Woolf; LEACH, Andrew; WO2011/121350; (2011); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia