HRID638637

反应详情

EQUATION

反应方程式

HRID 638637 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 10.2 g of dimethylcarbamyl chloride in 10 ml of methylene chloride is added dropwise to a mixture of 10.7 g of 2-(1,2-dichlorovinyloxy)phenylsulfonamide, 12.2 g of 1,8-diazabicyclo[5.4.0]undec-7-ene in 100 ml of methylene chloride at 20° to 25° C. and the mixture is refluxed for 2 hours. The solvent is then evaporated off and the residue is dissolved in 5% sodium carbonate solution. The solution is filtered and acidified with 10% hydrochloric acid, whereupon the product precipitates as crystals. After filtration and drying, 12.1 g of N-[2-(1,2-dichlorovinyloxy)phenylsulfonyl]-N',N'-dimethylurea are obtained. Melting point: 218°-220° C.

WORKUP

后处理

  1. temperaturethe mixture is refluxed for 2 hours
  2. customThe solvent is then evaporated off
  3. dissolutionthe residue is dissolved in 5% sodium carbonate solution
  4. filtrationThe solution is filtered
  5. customprecipitates as crystals
  6. filtrationAfter filtration
  7. customdrying