HRID1819454
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-[(quinolin-5-ylmethyl)-amino]-pyrimidin-4-ylamino}-methyl)-cyclohexyl]-carbamic acid tert-butyl ester (197 mg, 0.39 mmol) was dissolved in CH2Cl2 (10 mL) and TFA (2 mL) was added. The reaction mixture was stirred at room temperature for 1 h. The reaction mixture was treated with 3M Na2CO3 and the organic phase was separated. The organic phase was dried over Na2SO4 and concentrated. Silica gel purification using a mixture of 10:1:0.3 CH2Cl2:MeOH:Et3N yielded 120 mg of the title compound as a light yellow solid (79%), m/z 406.4 [M−1]+.
WORKUP
后处理
- customthe organic phase was separated
- dry with materialThe organic phase was dried over Na2SO4
- concentrationconcentrated
- customSilica gel purification
- additiona mixture of 10:1:0.3 CH2Cl2