HRID1169074
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
633 mg of ethyl 2-[3-chloro-6-[3-[4-(diphenylmethyl)-1-piperazinyl]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate trihydrochloride was dissolved in 6 ml of ethanol; 2.31 ml of a 2 N aqueous solution of sodium hydroxide was added, followed by thermal refluxing for 1.5 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 adjusted to pH 5 by the addition of 1 N hydrochloric acid. Methanol was added; the crystal precipitated was collected by filtration, washed with water-ethyl acetate and dried to yield 462 mg of the title compound.
WORKUP
后处理
- customrefluxing for 1.5 hours
- temperatureAfter cooling
- concentrationthe mixture was concentrated under reduced pressure
- additionThe residue was diluted with water
- washwashed with ethyl acetate
- additionthe water layer was adjusted to pH 5 by the addition of 1 N hydrochloric acid
- additionMethanol was added
- customthe crystal precipitated
- filtrationwas collected by filtration
- washwashed with water-ethyl acetate
- customdried