109-07-9, 2-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
A mixture of 1-CYCLOPROPYL-6, 7-difluoro-1, 4-DIHYDRO-8-METHOXY-4-OXO-3- quinoline carboxylic acid (100G), 2-methylpiperazine (67.8gs) and anhydrous DMSO (300 ml) were stirred for 40-45 hrs at 60-65C. The reaction mass was then diluted with 1500 ml isopropyl alcohol. It was then stirred for 30 min at 25-30C followed by cooling at 5 to 10 C along with stirring for 2 hours. The product was obtained by filtration, which was washed with 3 x 50 ml isopropyl alcohol followed by drying at 50 to 55C for 4 hours to provide 71 g Gatifloxacin (Yield 55. 9%) Example 2: Step A: A mixture of L-CYCLOPROPYL-6, 7-difluoro-1, 4-dihydro-8-methoxy-4-oxo-3- quinoline carboxylic acid (120Kg) 2-methylpiperazine (40.8 Kg), and anhydrous DMSO (361 lit) was heated to 60-65C temperature and stirred for 2 hrs. A second lot of 2-methylpiperazine (10.2 Kg) was added, and stirred for next 1 hr, at 60-65C. followed by the addition of a third lot of 2-methylpiperazine (10.2Kg). The mixture was stirred for next 2 hrs at 60-65C. A fourth lot of 2-methylpiperazine (20.4Kg) was added to the mixture and the stirring was continued for the next 24 hrs maintaining the temperature at 60-65C followed by cooling to 25-35C. This reaction mass was added in 1802-1 isopropyl alcohol. Reaction mass was then stirred for 30 min at 25- 30C followed by cooling at 5 to 10 C along with stirring for 2 hours. Product so obtained was centrifuged, washed with 3 x 60-1 isopropyl alcohol. The wet cake of PRODUCT WAS MIXED WITH 241-LIT METHANOL AND STIRRED FOR 1 HR. , AGAIN THE PRODUCT WAS centrifuged followed by washing with 59 lit of methanol. The wet Gatifloxacin was dried at 60 to 65C for 6 hrs to yield 81. 92 Kg dry Gatifloxacin (Yield= 53.7%) HPLC Purity = 99.74% M/C=3. 42%, 109-07-9
109-07-9 2-Methylpiperazine 66057, apiperazines compound, is more and more widely used in various fields.
Reference£º
Patent; CADILA HEALTHCARE LIMITED; WO2004/101527; (2004); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics