HRID1466055
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
A solution of Methyl ({2-[(tert-butoxycarbonyl)(7-cyano-1,2,3,4-tetrahydronaphthalen-2-yl)amino]ethyl}amino)acetate (145 mg, 0.37 mmol) in 15 mL of anhydrous DCM and 5 mL of TFA was stirred at room temperature for 2-3 hours. The reaction was concentrated. The residue was used directly in the next step. The residue was dissolved in 10 mL of EtOH, and was treated with TEA (5 mL). The mixture was heated to reflux overnight. The reaction was concentrated. The crude material was adsorbed onto silica gel and purified by MPLC (DCM:MeOH) to afford the title compound. MS m/z: 256 [M+1]+.
WORKUP
后处理
- concentrationThe reaction was concentrated
- dissolutionThe residue was dissolved in 10 mL of EtOH
- additionwas treated with TEA (5 mL)
- temperatureThe mixture was heated
- temperatureto reflux overnight
- concentrationThe reaction was concentrated
- custompurified by MPLC (DCM:MeOH)