HRID1746162

反应详情

EQUATION

反应方程式

HRID 1746162 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 2-isopropoxy-N-isopropyl-5-nitrobenzenamine 29 (385 mg, 1.62 mmol, 1 equiv) in ethanol (3 mL) was charged with 10% Pd/C (50% water, 253 mg, 0.162 mmol, 0.10 equiv) and air was evacuated with vacuum. The vacuum was replaced with a balloon filled with hydrogen gas, and the reaction was allowed to stir for 2 hours. The catalyst was filtered off using a pad of celite and rinsed with ethanol. The filtrate was concentrated, and the crude product was purified by flash chromatography and eluted with hexane:EtOAc=100:0 to 50:50 using 5% EtOAc increments to give 6-isopropoxy-N1-isopropylbenzene-1,3-diamine 31 (263 mg, 78%) as a solid.

WORKUP

后处理

  1. customwas evacuated with vacuum
  2. additionfilled with hydrogen gas
  3. filtrationThe catalyst was filtered off
  4. washrinsed with ethanol
  5. concentrationThe filtrate was concentrated
  6. customthe crude product was purified by flash chromatography
  7. washeluted with hexane