HRID1292949

反应详情

EQUATION

反应方程式

HRID 1292949 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixtre of 2-chloro-6-nitrobenzamide (0.3 g), iron powder (0.5 g) and t-butyl (N-2-oxoethyl)carbamate (1.0 g) in glacial acetic acid (5 mL) was heated at 50-55° C. for 2 h. The mixture was concentrated and the residue was partitioned between sat. NaHCO3 and EtOAc. The organic layer was dried (MgSO4), concentrated, and the residue was subjected to flash chromatography (silica gel/heptane-EtOAc 100:0 to 20:80 gradient) to afford the title compound as an off-white solid (0.1 g).

WORKUP

后处理

  1. concentrationThe mixture was concentrated
  2. customthe residue was partitioned between sat. NaHCO3 and EtOAc
  3. dry with materialThe organic layer was dried (MgSO4)
  4. concentrationconcentrated