Extracurricular laboratory: Synthetic route of 289042-12-2

According to the analysis of related databases, 289042-12-2, the application of this compound in the production field has become more and more popular.

Related Products of 289042-12-2, 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. 289042-12-2, name is tert-Butyl 2-((4R,6S)-6-((E)-2-(4-(4-fluorophenyl)-6-isopropyl-2-(N-methylmethylsulfonamido)pyrimidin-5-yl)vinyl)-2,2-dimethyl-1,3-dioxan-4-yl)acetate, molecular formula is C29H40FN3O6S, 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.

To a 3 L four-necked flask was added 1.5 L of absolute ethanol and 128.0 g of 6 – [(1E) -2- [4- (4-fluorophenyl) -6-isopropylYl-2- [methyl (methylsulfonyl) amino] -5-pyrimidine] vinyl] -2,3-dimethyl-1,3-dioxacyclohexane-4-acetic acid tert-butyl ester(Compound III). After stirring, 450 g of dilute hydrochloric acid solution with a mass fraction of 3.6% was added dropwise, stirred at room temperature for 4 to 6 hours, and TLC was monitored until compound III disappeared. After completion of the reaction, 320 g of a sodium hydroxide solution having a mass fraction of 4% was added dropwise to the reaction system and stirring was continued for 4 to 6 hours. The reaction was continued until the first stage of the dihydroxy ester intermediate was completely disappeared (residual?0.5%). The ethanol was then concentrated under reduced pressure, and then 2 L of purified water was added to the system. After stirring, the mixture was extracted twice with methyl t-butyl ether and the aqueous phase was concentrated to no organic solvent residue. The mass fraction was then slowly added to the resulting aqueous solution For 10% of the calcium acetate solution 420g, a white solid precipitation, after the drop is completed, continue stirring 4 to 6 hours, filtration, filter cake with 2L purified water beating 1 times, dry, filter cake vacuum drying, Statin calcium A, the yield was 87.0%, content ? 99.0%, purity(HPLC) ?99.0%, single maximum impurity ? 0.5%, product ee value ? 99.9%.

According to the analysis of related databases, 289042-12-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Anhui Mei Nuohua Pharmaceutical Chemical Co., Ltd.; Shi Jianxiang; Pan Qijiao; Ding Maohua; Gong Daoxin; Zhu Guosheng; (14 pag.)CN106674281; (2017); A;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia