HRID408858

反应详情

EQUATION

反应方程式

HRID 408858 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-((4-(4-Amino-3-fluorobenzoyl)piperazin-1-yl)methyl)-N-tert-butylfuran-2-carboxamide (Example 3; 0.05 g, 0.124 mmol) and N,N-diisopropylethylamine (0.028 mL) were dissolved in dichloromethane (5 mL). Bis(trichloromethyl)carbonate (0.014 g, 0.046 mmol) was added dropwise and the reaction was left to stir for 30 minutes. N,N-diisopropylethylamine (0.094 mL) was added to the reaction followed by 2-methylpropan-1-amine (0.018 g, 0.248 mmol, 0.025 mL) and the reaction was stirred for a further 2 hours. The reaction mixture was washed with water and flushed through a hydrophobic frit. The organic phase was concentrated under vacuum and purified by basic reverse phase HPLC to afford the title compound (5 mg).

WORKUP

后处理

  1. waitthe reaction was left
  2. stirringthe reaction was stirred for a further 2 hours
  3. washThe reaction mixture was washed with water
  4. customflushed through a hydrophobic frit
  5. concentrationThe organic phase was concentrated under vacuum
  6. custompurified by basic reverse phase HPLC