HRID2243331

反应详情

EQUATION

反应方程式

HRID 2243331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The procedure used in stage 1 of Example 1 is followed, but starting from 2.4 g of 3,4-diaminobenzonitrile and 30 ml of tetrahydrofuran, 4.6 ml of triethylamine and 4 g of fluoren-4-one-9-carboxylic acid chloride in 115 ml of dichloromethane. After stirring for 20 hours at room temperature, the precipitate that formed is filtered off, and washed with dichloromethane, with water, and then with a 10% saturated aqueous solution of sodium hydrogen carbonate and, finally, with water. After formation of a paste with diisopropyl ether, in this way we obtain 3.8 g of (2-amino-5-cyanophenyl)amide of 9-oxo-9H-fluorene-4-carboxylic acid, in the form of a beige powder, which is used as it is in the following stage, with the following characteristics:

WORKUP

后处理

  1. customthe precipitate that formed
  2. filtrationis filtered off
  3. washwashed with dichloromethane, with water