HRID1819469
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
(4-{[5-Nitro-2-(3-piperidin-1-yl-benzylamino)-pyrimidin-4-ylamino]-methyl}-cyclohexyl)-carbamic acid tert-butyl ester (176 mg, 0.33 mmol) was dissolved in CH2Cl2 (6 mL). To this solution was added TFA (3 mL) and the reaction was stirred for 1 h. The volatiles were removed and the crude was re-dissolved in 90:9:1 (CH2Cl2:CH3OH:NH4OH), then concentrated again to afford a solid. The resultant solid was purified via flash chromatography (SiO2, 10-75% CH2Cl2-(90:9:1-CH2Cl2:CH3OH:NH4OH)) to afford 131 mg (91%) of the target compound , m/z 440.72 [M+1]+.
WORKUP
后处理
- customThe volatiles were removed
- dissolutionthe crude was re-dissolved in 90:9:1 (CH2Cl2:CH3OH:NH4OH)
- concentrationconcentrated again
- customto afford a solid
- customThe resultant solid was purified via flash chromatography (SiO2, 10-75% CH2Cl2-(90:9:1-CH2Cl2:CH3OH:NH4OH))