60792-79-2, 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 60792-79-2 as follows.
Intermediate 20 6-(2-(2-Amino-ethoxyl-ethylamino(at)7-chloro-1-cyclopropyl-4-oxo-1,4-dihydro- quinoline-3-carboxylic acid (A) and 7-f 2-(2-Amino-ethoxy)-ethylaminol-1-cyclouropyl-6-flnoro-4-oxo-1,4-dihydro (at)uinoIine- 3-carboxylic acid (B) To a solution of 7-chloro-l-eyelopropyl-6-fluoro-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid (0.55g, 1.95 mmol) in 1-methyl-2-pyrrolidone (40 mL) bis-(2-aminoethyl)-ether dihydrochloride (2.1g, 11.9 mmol, 6eq. ) and DBU (3.49 mL, 23.4 mmol, 12 eq. ) added and the reaction mixture was stirred at 110 C for 18 hours. The reaction mixture was then diluted with water (70 mL), pH was adjusted to 11 and extracted with CH2Cl2 (9×40 mL). Water layer was then acified with H2S04 to pH 6.8, extracted with 50 mL of CH2C12 and then evaporated in vacuum. Crude product was diluted in 2-propanol (60 mL), stirred at 82 C for 20 minutes and filtrated. Precipitate was pure salt (Na2S04). 2-Propanol was evaporated in vacuum and product was purified by column chromatography (fraction, eluent: CH2C12- MeOH-NH3-CH3CN=4:4:2:1) yielding 0.5g of title compounds as a mixture of chloro and fluoro derivatives in ratio 3:1 MS (ES+) m/z : [MH] + = 365.8 (A) (75 %) MS (ES+) m/z : [MH] (at) = 349.4 (B) (25 %)
According to the analysis of related databases, 2,2′-Oxybis(ethylamine) dihydrochloride, the application of this compound in the production field has become more and more popular.
Reference:
Patent; PLIVA-ISTRAZIVACKI INSTITUT D.O.O.; WO2005/108413; (2005); A1;,
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