105-84-0

1204417-39-9

105-84-0

The general procedure for the synthesis of N,N',N''-trimethyldiethylenetriamine from the compound (CAS: 1204417-39-9) is as follows: Step 1: N,N-(2,2'-(methylureido)bis(ethane-2,1-diyl))bis(N-methyl-2-nitrobenzenesulfonamide) 7a (1.24 g, 2.405 mmol), cesium carbonate (2.35 g, 7.215 mmol, 3 eq.), and benzenethiol (795 mg, 7.215 mmol, 3 eq.) were dissolved in DMF (25 mL ) in DMF (25 mL) and the reaction was stirred at room temperature for 1 hour. Step 2: Upon completion of the reaction, the reaction mixture was filtered and the filtrate was upsampled onto an MP-TsOH column pre-washed with dichloromethane (DCM). Step 3: The cartridge was washed several times with DCM until the eluate was colorless, followed by elution of the target product with a methanol solution containing NH3. Step 4: The eluate was collected and concentrated to afford N,N'-dimethyl-N-(2-(methylamino)ethyl)ethane-1,2-diamine 7b (220 mg, 63% yield), which was used directly in the next step of the reaction; Mass Spectrum (m/z) = 146 (M + H)+.