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tert-butyl 3-(6-amino-1-methyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-5-ylamino)-2-methyl-3-oxopropylcarbamate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With dicyclohexyl-carbodiimide; In N,N-dimethyl-formamide; at 50℃; for 15h;Inert atmosphere;
To a mixture of 3-(tert-butoxycarbonylamino)-2-methylpropanoic acid (3.50 g,17.2 mmol) and <strong>[6972-82-3]5,6-diamino-1-methylpyrimidine-2,4(1H,3H)-dione</strong> (2.69 g, 17.2 mmol) inDMF (20 mL) was added DCC (10.66 g, 51.7 mmol). The reaction mixture was stirred at 50°C for 15h under N2 atmosphere. Water (50 mL) was added and the solid was removed byfiltration. The filtrate was concentrated in vacuo. The residue was purified by flash chromatography (MeOHIDCM= 1 / 10) to give tert-butyl 3 -(6-amino-i -methyl-2,4-dioxo- 1,2,3 ,4-tetrahydropyrimi din-5 -yl amino)-2-methyl -3 -oxopropylcarbamate: ESI: m/z 342.0 (M+H)tTo a solution of tert-butyl 3 -(6-amino-i-methyl -2,4-dioxo- 1,2,3 ,4-tetrahydropyrimidin-5 - ylamino)-2-methyl-3-oxopropylcarbamate (200 mg, 0.59 mmol) in EtOH (29 mL) was added aqueous NaOH (iN, 2.9 mL, 2.9 mmol). The mixture was heated to 50 °C and held at this temperature for i6h. Aqueous HC1 (iN) was added to pH5. The organic solvent was evaporated in vacuo and the aqueous residue was extracted with EA (20 mL*3). The combined organic fractions were concentrated. The residue was purified by flash column chromatography (DCM:MeOH =30:1) to give the title compound.
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