HRID224368

反应详情

EQUATION

反应方程式

HRID 224368 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

NH3 is passed into a refluxing solution of 1.48 g. of hexamethylenetetramine in 30 ml. of ethanol; 3.83 g. of 2-(α-bromo-α-fluoroacetamido)-5-nitro-2'-fluorobenzophenone, obtainable from 2-amino-5-nitro-2'-fluorobenzophenone and α-bromo-α-fluoroacetyl bromide, are added over 2 hours. The mixture is then heated under reflux for 3 hours more and is evaporated. The resulting 2-(α-amino-α-fluoroacetamido)-5-nitro-2'-fluorobenzophenone is treated with 15 ml. of toluene and 20 mg. of p-tolunesulfonic acid and is heated under reflux for 1 hour. Working up in the customary manner gives 3-fluoro-5-o-fluorophenyl-7-nitro-2,3-dihydro-1H-1,4-benzodiazepin-2-one.

WORKUP

后处理

  1. temperatureThe mixture is then heated
  2. temperatureunder reflux for 3 hours more
  3. customis evaporated
  4. additionThe resulting 2-(α-amino-α-fluoroacetamido)-5-nitro-2'-fluorobenzophenone is treated with 15 ml
  5. temperatureof p-tolunesulfonic acid and is heated
  6. temperatureunder reflux for 1 hour