HRID509184

反应详情

EQUATION

反应方程式

HRID 509184 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-thienyl-2-nitroaniline (1 equiv, 400 mg, 1.82 mmol) was added 10% Pd/C (0.05 equiv, 97 mg, 0.09 mmol). The resulting suspension was stirred for overnight over 1 atm of hydrogen. The solids were filtered through celite pad and the filtrate was concentrated under vacuum. The crude material was purified by silica gel column chromatography with gradient of MeOH (0-10%) in CH2Cl2 to afford compound 30 (310 mg, 90%) and a white solid. LRMS (ESI): (calc) 190.2 (found) 191.0 (MH)+.

WORKUP

后处理

  1. filtrationThe solids were filtered through celite pad
  2. concentrationthe filtrate was concentrated under vacuum
  3. customThe crude material was purified by silica gel column chromatography with gradient of MeOH (0-10%) in CH2Cl2