HRID261055
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
N,N'-dicyclohexylcarbodiimide (10.3 g; 0.05 moles) and 1-cyclohexylmethyl-4-aminopiperidine (9.8 g; 0.05 moles) were added successively to a solution of 2-methoxy-4-acetamido-5-chlorobenzoic acid (12.1 g; 0.05 moles) in methylene chloride (250 ml). After stirring overnight at room temperature, the insoluble N,N'-dicyclohexylurea was filtered off, the solution was washed with water, dried (Na2SO4) and the solvent removed in vacuo. The residue was recrystallized and the product converted into its hydrochloride to give 14.2 g of N-(1-cyclohexylmethylpiperid-4-yl)-2-methoxy-4-acetamido-5-chlorobenzamide hydrochloride monohydrate, m.p. 219°-221° C.
WORKUP
后处理
- filtrationthe insoluble N,N'-dicyclohexylurea was filtered off
- washthe solution was washed with water
- dry with materialdried (Na2SO4)
- customthe solvent removed in vacuo
- customThe residue was recrystallized