HRID2359393

反应详情

EQUATION

反应方程式

HRID 2359393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of 2-chloro-8-nitroquinoline (1.02 grams), iron powder (2.05 grams) and NH4Cl (2.6 grams) in 5:1 EtOH:Water (50 mL) was refluxed for 9 hours. After the reaction was complete, the solution was cooled to 60° C. and filtered through celite. The cake was washed with isopropyl alcohol followed by ethyl acetate. The filtrate was concentrated to dryness, dissolved in ethyl acetate and washed with water, dilute aqueous NaHCO3, brine and dried (Na2SO4) and concentrated to an oil. The desired product crystallized with the addition of pentane, brown solid (0.818 grams).

WORKUP

后处理

  1. filtrationfiltered through celite
  2. washThe cake was washed with isopropyl alcohol
  3. concentrationThe filtrate was concentrated to dryness
  4. dissolutiondissolved in ethyl acetate
  5. washwashed with water, dilute aqueous NaHCO3, brine
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated to an oil
  8. customThe desired product crystallized with the addition of pentane, brown solid (0.818 grams)