Reference of 13223-25-1 , The common heterocyclic compound, 13223-25-1, name is 2-Chloro-4,6-dimethoxypyrimidine, molecular formula is C6H7ClN2O2, 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.
4-(2-Bromophenyl)piperazine-1-carboxylic acid tert-butyl ester (280 mg, 0.82 mmol),4,6-Dimethylpyrimidin-2-amine (151 mg, 1.23 mmol),Sodium tert-butoxide (0.16 g, 1.16 mmol), tris(dibenzylideneacetone) dipalladium (75 mg, 0.082 mmol) and(±)-2,2′-bis-(diphenylphosphino)-1,1′-binaphthyl (102 mg, 0.164 mmol) was added to anhydrous tolueneIn (20 mL), the reaction was heated to 120 C for 12 hours under a nitrogen atmosphere. The reaction was stopped, and the mixture was cooled to room temperature. The mixture was poured into water (100 mL), ethyl acetate (40 mL×3), and the organic phase was combined and washed with water (50 mL) and brine (50 mL) Dry and distill off the solvent under reduced pressure.The obtained crude product was subjected to column chromatography (dichloromethane:methanol (V:V)=50:1)The title compound (white solid, 274 mg, 87%)
The synthetic route of 13223-25-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Jin Chuanfei; Zhang Yingjun; Xue Yaping; Guo Zhengjiang; (39 pag.)CN109912514; (2019); A;,
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