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. 1374639-78-7, name is tert-Butyl 4-(6-((7-cyclopentyl-6-(dimethylcarbamoyl)-7H-pyrrolo[2,3-d]pyrimidin-2-yl)amino)pyridin-3-yl)piperazine-1-carboxylate, molecular formula is C28H38N8O3, 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. HPLC of Formula: C28H38N8O3
A solution of tert-butyl 4-(6-((7-cyclopentyl-6-(dimethylcarbamoyl)-7H-pyrrolo[2,3- d]pyrimidin-2-yl)amino)pyridin-3-yl)piperazine-l-carboxylate (Ila) (50 g) in toluene (300 mL) was cooled to 10 C. Hydrochloric acid (6N, 100 mL) was added to the above solution in drop wise at 15 C. The reaction mass was stirred for 1 hour at 25-30 C. Hydrochloric acid (IN, 200 mL) was added to the above reaction mass at 25-30 C and stirred for 10 minutes at the same temperature. The reaction mass was then filtered and washed with toluene (1 x 50 mL) followed by hydrochloric acid (IN, 50 mL). Organic layer was separated and aqueous layer was cooled to 15 C. pH of aqueous layer was adjusted to pH=12.0-12.5 using saturated solution of sodium hydroxide (50% w/w) and stirred for 1 hour at 15-20 C. The resulted precipitate was then filtered, washed with water (3 chi 80 mL) and dried at 50 C for 6 hours to provide the title compound. (0169) Yield: 35.1 g; Purity by HPLC: 99.31 %
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Reference:
Patent; DR. REDDY?S LABORATORIES LIMITED; PEDDIREDDY, Subba Reddy; KOTTUR, Mohan Kumar; ORUGANTI, Srinivas; KANDAGATLA, Bhaskar; DAS GUPTA, Shirshendu; (39 pag.)WO2018/51280; (2018); A1;,
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