HRID1834718

反应详情

EQUATION

反应方程式

HRID 1834718 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

40.2 g. of N-(β-hydroxyethyl)-benzene sulfonamide was slurried in 100 ml. of carbon tetrachloride containing 5 drops of piperidine. Then, 47.6 g. of sulfonyl chloride was added over 10 minutes, keeping the temperature at 20°-25° C. during the addition. The reaction was completed by heating on a steam bath for 1 hour. The mixture was concentrated on the steam bath, dissolved in benzene and washed twice with dilute aqueous solution of sodium chloride, dried over magnesium sulfate, filtered and the benzene evaporated on the steam bath with air. The product was crystallized from benzene cyclohexane to yield 28.0 g. of product, m.p. 58°-62° C.

WORKUP

后处理

  1. customat 20°-25° C.
  2. additionduring the addition
  3. temperatureby heating on a steam bath for 1 hour
  4. concentrationThe mixture was concentrated on the steam bath
  5. dissolutiondissolved in benzene
  6. washwashed twice with dilute aqueous solution of sodium chloride
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. customthe benzene evaporated on the steam bath with air
  10. customThe product was crystallized from benzene cyclohexane
  11. customto yield 28.0 g