HRID979609

反应详情

EQUATION

反应方程式

HRID 979609 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

A mixture of 23.2 g (0.10 mole) of 2-amino-4'-chlorobenzophenone and 14.7 g (0.11 mole) of 3-amino-2-chloropyridine (96%) were heated for 1.5 hr at 180° C. under nitrogen atmosphere. The mixture was cooled to room temperature and methylene chloride added. After stirring for 30 min., solids were separated by filtration and triturated in hot 190 proof ethanol. The remaining insoluble material was collected by filtration and recrystallized from benzene-isooctane to give 2.7 g product, m.p. 203°-204.5° C. Drying conditions prior to analyses were: overnight at 97°-98° C./0.1 mm Hg.

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. customsolids were separated by filtration
  3. customtriturated in hot 190 proof ethanol
  4. filtrationThe remaining insoluble material was collected by filtration
  5. customrecrystallized from benzene-isooctane