HRID2049909

反应详情

EQUATION

反应方程式

HRID 2049909 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred solution of 12.8 g. of nitrotrimesic acid (prepared by alkaline potassium permanganate oxidation of nitromesitylene) in 200 ml. of water containing 30 g. of sulfuric acid are added 6.5 g. of zinc dust in portions at such a rate so as to maintain a temperature of about 25° C. After the addition, the mixture is stirred for an additional 1 hr. After this time, 200 ml. of ethyl acetate are added and the mixture is rapidly stirred for 15 min. The reaction is then filtered by suction through a pad of filter aid. The organic layer is separated, dried and concentrated under reduced pressure, leaving 9.6 g. of crude product which is used directly in the next step. ##STR15##

WORKUP

后处理

  1. additionAfter the addition
  2. stirringthe mixture is rapidly stirred for 15 min
  3. filtrationThe reaction is then filtered by suction through a pad of filter aid
  4. customThe organic layer is separated
  5. customdried
  6. concentrationconcentrated under reduced pressure
  7. customleaving 9.6 g