HRID366978

反应详情

EQUATION

反应方程式

HRID 366978 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 4-amino-1-naphthalene sulfonic acid (200 g, 0.897 mole) in 800 ml of pyridine was stirred mechanically while methanesulfonyl chloride (70 ml, 0.9 mole) was added slowly over about 10 min. The reaction warmed to about 60° as the solid dissolved and then slowly cooled to room temperature. The mixture was stirred overnight while a solid precipitated. After filtering and washing with 500 ml of ether, the solid was dried under a nitrogen stream to afford 211 g (62%) of 4-methanesulfonamido-1-naphthalene sulfonic acid pyridinium salt.

WORKUP

后处理

  1. additionwas added slowly over about 10 min
  2. temperatureThe reaction warmed to about 60° as the solid
  3. dissolutiondissolved
  4. customprecipitated
  5. filtrationAfter filtering
  6. washwashing with 500 ml of ether
  7. customthe solid was dried under a nitrogen stream