HRID1589423

反应详情

EQUATION

反应方程式

HRID 1589423 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 250 ml round bottomed flask is placed 90 ml of N,N-dimethylformamide and 30 grams (0.092 mole) of 3-amino sulfonyl-4-chlorobenzhydrazide. The mixture was stirred to dissolve the solid, then 18.63 gms (0.138 mole) of crotyl bromide were added. The mixture was heated at 100° for 1.66 hours at which point TLC showed the reaction to be complete. The reaction mixture was cooled and diluted with 200 ml isopropanol. This solution was dripped into a slurry of 1.5 liters of ice and 4 liters of water. The solid which precipitated was collected, washed with water and air dried overnight, yielding the product which could be recrystallized from chloroform/carbon tetrachloride.

WORKUP

后处理

  1. customIn a 250 ml round bottomed flask is placed
  2. dissolutionto dissolve the solid
  3. temperatureThe mixture was heated at 100° for 1.66 hours at which point TLC
  4. customthe reaction
  5. temperatureThe reaction mixture was cooled
  6. customThe solid which precipitated
  7. customwas collected
  8. washwashed with water and air
  9. customdried overnight
  10. customyielding the product which
  11. customcould be recrystallized from chloroform/carbon tetrachloride