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tert-butyl (2-(4-(2-hydroxy-2-methylpropyl)piperazin-1-yl)ethyl)carbamate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
73%
With potassium carbonate; sodium iodide; In N,N-dimethyl-formamide; at 70 - 80℃; for 24h;
To a solution of tert-butyl (2-(piperazin-1-yl)ethyl)carbamate (1 g, 4.4 mmol) in DMF (15 mL) was added 1-chloro-2-methylpropan-2-ol (1.89 g, 17.4 mmol), K2C03 (1.8 g, 13.1mmol) and Nal (1.31 g, 8.7 mmol). The reaction was stirred at 70-80 °C for 24 h, cooled to room temperature, and poured into water. The reaction mixture was extracted with ethyl acetate, and the organic layers were combined, washed with brine, dried (Na2SO4), filtered and concentrated. The crude residue was chromatographed (silica gel, DCM : MeOH = 40 : 1) to afford tert-butyl (2-(4-(2-hydroxy-2-methylpropyl)piperazin- 1 -yl)ethyl)carbamate as an oil (0.95 g, 73percent).
With N-ethyl-N,N-diisopropylamine; In acetonitrile; for 8h;Reflux;
The product from step b of this example (0.74 g, 3.2 mmol), propargyl-peg4-tosylate (1.9 g, 4.8 mmol), and diisopropylethylamine (0.83 g, 6.5 mmol) were stirred in acetonitrile (20 ml) at reflux for 8 hours. The mixture was cooled and purified by reverse phase liquid chromatography (RPLC) using an Isco CombiFlash liquid chromatograph eluted with 5% to 80% acetonitrile/water with 0.1% TFA as the modifier, 30 minute gradient. The pure fractions were pooled and concentrated to afford the product as a thick light yellow oil. Yield 0.71 g, 50%. LC/MS [M+H]+ = 444.2.
Chemistry
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