HRID371476

反应详情

EQUATION

反应方程式

HRID 371476 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 38.9 g (0.20 mole) of 4-fluorobenzenesulfonylchloride in 20 ml of methylene chloride was added slowly to 300 ml of a 40% aqueous dimethylamine solution during 0.5 hour period. The reaction was exothermic. After the reaction mixture was cooled a yellow solid was precipitated. The solid was collected, dissolved in 300 ml of ethyl acetate, and dried over magnesium sulfate. The solution was concentrated to 100 ml and a light yellow crystal formed. The crystal was collected and air-dried to afford 39 g of the product, mp 40°-43° C.

WORKUP

后处理

  1. temperatureAfter the reaction mixture was cooled a yellow solid
  2. customwas precipitated
  3. customThe solid was collected
  4. dissolutiondissolved in 300 ml of ethyl acetate
  5. dry with materialdried over magnesium sulfate
  6. concentrationThe solution was concentrated to 100 ml
  7. customa light yellow crystal formed
  8. customThe crystal was collected
  9. customair-dried