HRID1067571

反应详情

EQUATION

反应方程式

HRID 1067571 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.85 g of isopropyl [6-[3-[4-(diphenylmethoxy) piperidino]propoxy][1,2,4]triazolo[1,5-b]pyridazin-2-yl]carboxylate was dissolved in 18 ml of tetrahydrofuran; 3.8 ml of a 1 N aqueous solution of sodium hydroxide was added, followed by stirring at room temperature for 3.5 hours. After cooling, the mixture was concentrated under reduced pressure; the residue was diluted with water and washed with ethyl acetate; 1 N hydrochloric acid was added to ajust pH 4.5. The mixture was crystallized by the addition of ethanol-acetone (1:2), collected by filtration, washed with water and ethyl acetate and dried to yield 1.33 g of the title compound.

WORKUP

后处理

  1. temperatureAfter cooling
  2. concentrationthe mixture was concentrated under reduced pressure
  3. additionthe residue was diluted with water
  4. washwashed with ethyl acetate
  5. addition1 N hydrochloric acid was added to ajust pH 4.5
  6. customThe mixture was crystallized by the addition of ethanol-acetone (1:2)
  7. filtrationcollected by filtration
  8. washwashed with water and ethyl acetate
  9. customdried