HRID436688

反应详情

EQUATION

反应方程式

HRID 436688 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-(((3,6-dichloro-2-pyridinyl)methyl)thio)benzenamine (10 grams; 0.035 mole) in 25 ml. of dry pyridine was prepared and dimethyl carbamoyl chloride (3.77 grams; 0.035 mole) added thereto while maintaining the temperature of the reaction mixture at 24°-45° C. The resulting reaction mixture was stirred at ambient temperatures for a period of about 15 hours and then mixed with ice and allowed to stand for a period of about two hours. The aqueous layer was decanted and the residue washed with water and recrystallized twice from ether. As a result of the above operations, the desired N'-(4-(((3,6-dichloro-2-pyridinyl)methyl)thio)phenyl)-N,N-dimethyl urea compound was recovered as a crystalline solid having a melting point of 112°-113.5° C.

WORKUP

后处理

  1. temperaturewhile maintaining the temperature of the reaction mixture at 24°-45° C
  2. customThe resulting reaction mixture
  3. additionmixed with ice
  4. waitto stand for a period of about two hours
  5. customThe aqueous layer was decanted
  6. washthe residue washed with water
  7. customrecrystallized twice from ether
  8. customAs a result of the above operations
  9. customthe desired N'-(4-(((3,6-dichloro-2-pyridinyl)methyl)thio)phenyl)-N,N-dimethyl urea compound was recovered as a crystalline solid