HRID361812
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
A mixture of 1-benzyl-4-(methylamino)piperidine (EXAMPLE 9, 2.92 g) and 2-bromo-3-ethoxypyridine (EXAMPLE 69, 1.44 g) is stirred at 160°-165° in a sealed tube for 2 days, diluted with methylene chloride (50 ml), washed with water (10 ml) and saline (10 ml), dried over sodium sulfate, and concentrated under reduced pressure. The residue is chromatographed on silica gel (230-400 mesh, 300 g; eluting with a gradient of ethyl acetate/hexane (10/90-50/50)) to give the title compound, C,H,N: Anal. Calcd for C20H27N3O1 : C=73.81, H=8.36, N=12.91-found: C=73.59, H=8.37, N=12.83.
WORKUP
后处理
- washwashed with water (10 ml) and saline (10 ml)
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue is chromatographed on silica gel (230-400 mesh, 300 g
- washeluting with a gradient of ethyl acetate/hexane (10/90-50/50))