HRID1857355

反应详情

EQUATION

反应方程式

HRID 1857355 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-chloro-5-ethylphenylcyanamide (0.6 g, 3.08 mmol), 3-ethylaniline mesylate (0.64 g, 2.93 mmol), and chlorobenzene (12 mL) were combined in a dry round bottom flask equipped with a water cooled condenser under nitrogen and placed in a preheated oil bath (150-160° C.). The reaction mixture was heated for 3 hours. After cooling, the crude reaction product was purified by crystallization from chlorobenzene/diethylether. The resulting crystals were collected by filtration, washed with diethylether, and dried in a vacuum oven (40° C., 15 hours) to yield the title compound, N-(3-ethylphenyl)-N'-(2-chloro-5-ethylphenyl)guanidine mesylate, as a white solid (1.1 g, 91% yield).

WORKUP

后处理

  1. customwere combined in a dry round bottom flask
  2. customequipped with a water cooled condenser under nitrogen
  3. customplaced in a preheated oil bath
  4. custom(150-160° C.)
  5. temperatureThe reaction mixture was heated for 3 hours
  6. temperatureAfter cooling
  7. customthe crude reaction product
  8. customwas purified by crystallization from chlorobenzene/diethylether
  9. filtrationThe resulting crystals were collected by filtration
  10. washwashed with diethylether
  11. customdried in a vacuum oven (40° C., 15 hours)