Downstream synthetic route of 109-07-9

109-07-9, As the paragraph descriping shows that 109-07-9 is playing an increasingly important role.

109-07-9, 2-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example of preparation. Preparing form I gatifloxacin for seeding; 10 g (0.0339 moles, 1 equivalent) of 1- cyclopropyl-6, 7-difluoro-1, 4-dihydrc-8-methoxy-4-oXo-3- quinolinecarboxylic acid (CAS no.: 112811-72-0) is placed in a flask, 30 mL of acetonitryl (3 volumes) is added and the solution is heated to a temperature of 76-80 C. Once reflux has been attained, 3.28 g (0.0203 moles, 0.6 equivalents) of hexamethyldisilazane (HMDS) is added using a compensated addition funnel, maintaining the temperature. Once the addition is completed, the reaction is maintained with stirring for 1 hour at a temperature of 76-80 C. Once this period has elapsed, the reaction mixture is cooled to a temperature between 0 and 15 C, and 5.78 g (0.0407 moles, 1.2 equivalents) of boron trifluoride ethyletherate is added, keeping the temperature below 15 C. Once the addition has finished, the temperature is allowed to rise to 15-25 C and :-t is kept under these conditions for approximately 2 hour : :. The pH of the mixture is then adjusted to an approximate value of 9 with triethylamine (approximately 2 mL). To the resulting suspension : s added a solution of 10.19 g (0.1017 moles, 3 equivalents) of 2-methylpiperazine in 28 mL of acetonitryl, keeping the temperature between 15 and 25 C. The resulting amber solution is kept with stirring under these conditions for approximately 3 hours. Once the reaction has beer : completed, the mixture is distilled at low pressure unti : a stirrable paste is obtained. At this point, 50 mL of methanol is added, the resulting suspension is raised to a temperature of 63-67 C and kept under these conditions for approximately 5 hours. Once the reaction has been completed the mixture is cooled to a temperature of 25-35 C over a water bath and then to a temperature of 0-5 C over a water/ice bath for a further 1 hour. The resulting precipitate is filtered, washed with cold methanol (2 x 10 mL) and dried at 40 C in an oven in vacuo to constant weight. 10.70 g of crude gatifloxacin is obtained, with a water content of 2. 95% by weight. The yield of the process is 81.8%. The crude product obtained is used for the seeding in Example 1. The crude product is crystallised in methanol by dissolving-20 g of crude gatifloxacin in 1 1 of methanol (50 volumes) at a temperature of D3-67 C. Once all the product has been dissolved it is placed to cool to a temperature of 30-40 C, and then to a temperature of 0-5 C over a water/ice bath, maintaining it under these conditions for 1 hour. The resulting suspension is filtered and the solid retained is washed with 20 mL (1 volume) of cold methanol. The solid obtained is dried at 40 C in a vacuum oven to obtain 18.65 g of gatifloxacin with a water content of 2. 36% by weight.

109-07-9, As the paragraph descriping shows that 109-07-9 is playing an increasingly important role.

Reference£º
Patent; QUIMICA SINTETICA, S.A.; WO2005/47262; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics