HRID1466055

反应详情

EQUATION

反应方程式

HRID 1466055 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. concentrationThe reaction was concentrated
  2. dissolutionThe residue was dissolved in 10 mL of EtOH
  3. additionwas treated with TEA (5 mL)
  4. temperatureThe mixture was heated
  5. temperatureto reflux overnight
  6. concentrationThe reaction was concentrated
  7. custompurified by MPLC (DCM:MeOH)