HRID27777

反应详情

EQUATION

反应方程式

HRID 27777 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

12 ml of pyridine was added to 0.4 g of 5-(1-hydroxy-2-isopropylaminobutyl)-8-hydroxycarbostyril, and 0.6 ml of isobutyryl chloride was added dropwise to the mixture while cooling with ice-water and stirring followed by stirring for 3 hours. After addition of about 200 ml of diethyl ether, the precipitate formed was washed thoroughly with diethyl ether and dissolved in 50 ml of water. The solution was washed with dichloroethane and the aqueous layer was concentrated to dryness. Acetone was added to the residue to crystallize the product which was then recrystallized from acetone to obtain 0.33 g of 5-(1-hydroxy-2-isopropylaminobutyl)-8-isobutyryloxycarbostyril hydrochloride having a melting point of 228°-229° C. (with coloration and decomposition).

WORKUP

后处理

  1. additionwas added dropwise to the mixture
  2. stirringby stirring for 3 hours
  3. customthe precipitate formed
  4. washwas washed thoroughly with diethyl ether
  5. dissolutiondissolved in 50 ml of water
  6. washThe solution was washed with dichloroethane
  7. concentrationthe aqueous layer was concentrated to dryness
  8. additionAcetone was added to the residue
  9. customto crystallize the product which
  10. customwas then recrystallized from acetone