HRID1878392

反应详情

EQUATION

反应方程式

HRID 1878392 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 3-((4-(4-amino-3-fluorobenzoyl)-2-(fluoromethyl)piperazin-1-yl)-methyl)-N-tert-butylbenzamide (150 mg, 0.34 mmol) in dichloromethane (4 mL) at room temperature was added 4-nitrophenyl chloroformate (71.4 mg, 0.354 mmol). The reaction mixture was stirred at room temperature for 1 hour before the addition of cyclopropane-methylamine (150 μL). The mixture was stirred at room temperature overnight before being applied to a silica carbonate column. The eluant was concentrated under reduced pressure and redissolved in methanol. Purification by basic reverse phase HPLC gave the title compound (2 mg), MS (ESI) m/z 542.5 [M+H]+

WORKUP

后处理

  1. concentrationThe eluant was concentrated under reduced pressure
  2. dissolutionredissolved in methanol
  3. customPurification by basic reverse phase HPLC