HRID1067540
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
653 mg of ethyl 2-[3-chloro-6-[3-[4-(diphenylmethoxy)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate dihydrochloride was dissolved in 6 ml of ethanol; 1.97 ml of a 2 N aqueous solution of sodium hydroxide was added, followed by thermal refluxing for 2.5 hours. After cooling, the mixture was concentrated under reduced pressure; the residue was diluted with water and washed with ethyl acetate; the water layer was ajusted to pH 4.5 by the addition of 1 N hydrochloric acid. Acetone was added; the crystal precipitated was collected by filtration, washed with water-acetone (5:1) and dried to yield 465 mg of the title compound.
WORKUP
后处理
- customrefluxing for 2.5 hours
- temperatureAfter cooling
- concentrationthe mixture was concentrated under reduced pressure
- additionthe residue was diluted with water
- washwashed with ethyl acetate
- additionthe water layer was ajusted to pH 4.5 by the addition of 1 N hydrochloric acid
- additionAcetone was added
- customthe crystal precipitated
- filtrationwas collected by filtration
- washwashed with water-acetone (5:1)
- customdried