HRID1258752

反应详情

EQUATION

反应方程式

HRID 1258752 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of (S)—N-(4-chloro-3-(3-(4-chloro-5-(2-(methoxymethyl)pyrrolidin-1-yl)-2-nitrophenyl)thioureido)benzyl)-1-(trifluoromethyl)cyclopropanecarboxamide (145 mg; 0.23 mmol), Fe (65 mg; 1.2 mmol), saturated aqueous NH4Cl-solution (3 mL) and EtOH (3 mL) was stirred at 90° C. for 2 h. The mixture was basicified to pH-9-10 and filtered through celite. The celite pad was washed with EtOH and EtOAc. The mixture was concentrated and the residue was extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was washed with Et2O to give the sub-title compound.

WORKUP

后处理

  1. filtrationfiltered through celite
  2. washThe celite pad was washed with EtOH and EtOAc
  3. concentrationThe mixture was concentrated
  4. extractionthe residue was extracted with EtOAc
  5. dry with materialThe organic layer was dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. washThe residue was washed with Et2O