HRID1763574

反应详情

EQUATION

反应方程式

HRID 1763574 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

An 86.3 g sample of 6-(p-bromophenyl)-4,5-dihydro-3-(2H)-pyridazinone (prepared as in U.S. Pat. No. 3,689,652 Example 5) is dissolved in 500 ml. of glacial acetic acid by heating to 80° C. with continuous stirring. A solution of 60 g. of bromine in 80 ml. of acetic acid is added dropwise at 75°-80° C over a 1 hour period. A solid is separated near the end of the addition. The reaction mixture is heated with stirring on the steam bath for half an hour mote, then is poured into 3 liters of cracked ice-water. The white solid formed is collected by filtration and is air dried. The product is then recrystallized from ethyl alcohol to afford 6-(p-bromophenyl)-3(2H)-pyridazinone.

WORKUP

后处理

  1. dissolution3,689,652 Example 5) is dissolved in 500 ml
  2. customA solid is separated near the end of the addition
  3. temperatureThe reaction mixture is heated
  4. additionis poured into 3 liters of cracked ice-water
  5. customThe white solid formed
  6. filtrationis collected by filtration
  7. customdried
  8. customThe product is then recrystallized from ethyl alcohol