With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.3022-15-9,Piperazine-2-carboxylic acid dihydrochloride,as a common compound, the synthetic route is as follows.
Piperazine-2-carboxyilc acid dihydrochloride (5.00 g, 24.6 mmol) was dissolved in H2O (80 mL) and 1,4-dioxane (80 mL), and the solution was brought to pH 11 with 50% aqueous NaOH. A solution of di-tert-butyl dicarbonate (5.36 g, 30.8 mmol) in 1,4-dioxane (40 mL) was added dropwise while maintaining the pH at 11 with 50% aqueous NaOH. After 12 h, the reaction mixture was extracted with Et2O (3 x 125 mL). The aqueous layer was brought to pH 2 with concentrated HCl and was extracted with EtOAc (4 x 100 mL). The aqueous solution was brought to pH 9.5 with 50% aqueous NaOH. Benzyl chloroformate (3.70 mL, 24.6 mmol) was added at 10 0C while maintaining the pH at 9.5 with 50% aqueous NaOH. The solution was allowed to warm to rt. After 2 h, the reaction mixture was extracted with Et2O (2 x 100 mL), brought to pH 1 with concentrated HCl, and extracted with EtOAc (3 x 150 mL). The combined EtOAc extracts were dried over Na2SO4, filtered, and concentrated under reduced pressure. The thick oil was dissolved in THF (100 mL) and cooled to 00C. Borane-THF complex (1.0 M solution in THF, 75 mL, 75 mmol) was added portionwise. After 1 h, the reaction mixture was heated to 50 0C. After 1 h, the
3022-15-9, The synthetic route of 3022-15-9 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; CRITICAL THERAPEUTICS, INC.; WO2007/146066; (2007); A2;,
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