Reference of 69785-94-0, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 69785-94-0 as follows.
Step 2. 3-{2-cyano-1-[4-(7-{[2-(trimethylsilyl)ethoxy]methyl}-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrazol-1-yl]ethyl}-N-(4-hydroxypyrimidin-5-yl)pyrrolidine-1-carbothioamide5-Aminopyrimidin-4-ol (52.4 mg, 0.203 mmol) was dissolved in pyridine (0.55 mL) and phenyl chlorothionocarbonate (33 microL, 0.24 mmol) was added. The mixture was stirred at RT for one h. The reaction was diluted with DCM and washed with water and brine, the organic phase was dried over sodium sulfate and concentrated. The residue was dissolved in chloroform (1.7 mL), and triethylamine (141 microL, 1.01 mmol) and 3-pyrrolidin-3-yl-3-[4-(7-{[2-(trimethylsilyl)ethoxy]methyl}-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrazol-1-yl]propanenitrile (75 mg, 0.17 mmol; from Example 15, Step 3) were added. The mixture was stirred for 30 min at 70 C. The solvents were removed in vacuo and the product was purified by preparative-HPLC/MS (C18 column eluting with a gradient of ACN/H2O containing 0.15% NH4OH) (15 mg, 15%). LCMS (M+H)+: 591.1.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,69785-94-0, its application will become more common.
Reference:
Patent; Rodgers, James D.; Shepard, Stacey; Arvanitis, Argyrios G.; Wang, Haisheng; Storace, Louis; Folmer, Beverly; Shao, Lixin; Zhu, Wenyu; Glenn, Joseph; US2010/298334; (2010); A1;,
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