Electric Literature of 13036-57-2 , The common heterocyclic compound, 13036-57-2, name is 2-Chloro-4-methylpyrimidine, molecular formula is C5H5ClN2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
To a solution of ethyl 3-{[(2,6-diotafluorophenyl)sulfonyl]amiotano}-4-fluorobenzoate (5 0 g, 13 9 mmol) in THF (100 mL) was added 1 0 M LHMDS in THF (34 8 mL, 34 8 mmol) A solution of 2-chloro-4-methylpyriotamiotadiotane (2 7 g, 20 9 mmol) in THF (100 mL) was added dropwise over 30 mm, and the reaction was stirred overnight at rt The reaction was quenched with 10 mL of MeOH and concentrated, and the residue was partitioned between EtOAc and saturated aqueous sodium bicarbonate The aqueous layer was extracted with 2×50 mL EtOAc, and the combined organic layers were passed through a pad of silica gel, concentrated, and adsorbed onto silica gel The crude product was purified via flash chromatography with 0-100% EtOAc/DCM to generate 3 07 g (50% yield) of the product of Step B as a white powder ES- LCMS m/z 443 (M+H)
The synthetic route of 13036-57-2 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; GLAXOSMITHKLINE LLC; ADJABENG, George; BAUM, Erich; BIFULCO, Neil; DAVIS-WARD, Ronda, G.; DICKERSON, Scott, Howard; DONALDSON, Kelly, Horne; HORNBERGER, Keith; PETROV, Kimberly; RHEAULT, Tara, Renae; SAMMOND, Douglas, McCord; SCHAAF, Gregory, M.; STELLWAGEN, John; UEHLING, David, Edward; WATERSON, Alex, Gregory; WO2010/104899; (2010); A1;,
Pyrimidine | C4H4N2 – PubChem,
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