HRID1258748

反应详情

EQUATION

反应方程式

HRID 1258748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of N-(3-nitro-4-trifluoromethoxy-benzyl)-2,2-dimethyl-propionamide (3.4 g, 11 mmol), Fe (3.7 g, 66 mmol), saturated aqueous NH4Cl-solution (35 mL) and EtOH (170 mL) was refluxed for 30 min. The mixture was concentrated, treated with water and the pH was adjusted to ˜8. The mixture was extracted with EtOAc and the organic layer was dried over Na2SO4, filtered and concentrated. The residue was treated with PE and the sub-title compound was filtered off. Yield: 2.7 g (88%).

WORKUP

后处理

  1. temperaturewas refluxed for 30 min
  2. concentrationThe mixture was concentrated
  3. additiontreated with water
  4. extractionThe mixture was extracted with EtOAc
  5. dry with materialthe organic layer was dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. additionThe residue was treated with PE
  9. filtrationthe sub-title compound was filtered off