929-75-9, 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. 929-75-9 name is 1,11-Diamino-3,6,9-trioxaundecane, This 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.
N-i^e-Dichlorotl^^Jtriazin^-y -HO-dimethyl-hydroxylamine (XXX) (1.63 g, 7.8 mmol) in EtOH (100 mL) was added to 2,2′-(2,2*-oxybis(ethane- 2,l-diyl)bis(oxy))diethanamine {Org. Biomol. Che . 2005, 3:2255-61) (1.5 g, 7.8 mmol) and DIPEA (2.01 g, 15.6 mmol). The reaction was heated at 100 C for 3 h, after which time the solvent was removed under reduced pressure. The residue was dissolved in EtOAc (200 mL), washed with water (2 x 100 mL) and then with a brine solution (100 mL) and lastly dried over Na2S0 . The solvent was removed under reduced pressure and the residue was purified by flash column chromatography (DCM MeOH=50/l to 20/1) to yield N-(5,8,l l-trioxa-2, 14,16,18,19- pentaazabicyclo[l 3.3.1 ]nonadeca-l(l 8), 15( 1 ), 16( 17)-trien-l 7-yl)-N,0- dimethylhydroxylamine (CXVII) (700 mg) as a colourless oil (yield 27%).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,11-Diamino-3,6,9-trioxaundecane, and friends who are interested can also refer to it.
Reference:
Patent; GALLEON PHARMACEUTICALS, INC.; DAX, Scott, L.; WOODWARD, Richard; PENG, Sean; WO2012/74999; (2012); A1;,
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