反应详情

温度

25 °C

N4-{[Trans-4-(3-aminoazetidin-1-yl)cyclohexyl]methyl}-5-nitro-N2-[2-(trifluoromethoxy)benzyl]pyrimidine-2,4-diamine (20 mg, 0.04 mmol) was dissolved in CH2Cl2 (1.0 mL). To this solution was added acetic anhydride (0.057 mL, 0.06 mmol) followed by triethylamine (0.084 mL, 0.06 mmol). The reaction was allowed to stir at 25° C. for 18 h. The volatiles were removed and the crude was redissolved in CH2Cl2 and extracted with 10% aqueous NaHCO3. The aqueous phase was separated and extracted two more times with CH2Cl2. The organic layers were combined, dried (Na2SO4), decanted and concentrated. The resultant residue was purified via flash chromatography (SiO2, 10-30% (2:18:80, NH4OH:CH3OH:CH2Cl2)—CH2Cl2) to afford 16 mg (74%) of the target compound, m/z 538.46 (M+1)+.

1. customThe volatiles were removed
2. dissolutionthe crude was redissolved in CH2Cl2
3. extractionextracted with 10% aqueous NaHCO3
4. customThe aqueous phase was separated
5. extractionextracted two more times with CH2Cl2
6. dry with materialdried (Na2SO4)
7. customdecanted
8. concentrationconcentrated
9. customThe resultant residue was purified via flash chromatography (SiO2, 10-30% (2:18:80, NH4OH:CH3OH:CH2Cl2)—CH2Cl2)