HRID899147
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
To a suspension of N-(2-bromoethyl)-N-[2-(4-cyanophenoxy)ethyl]methane-sulfonamide (6 g, 0.019 mol; see Preparation C above) and anhydrous potassium carbonate (3.6 g, 0.026 mol) in dry acetonitrile (100 mL) was added 9-oxa-3,7-diaza-bicyclo[3.3.1]nonane-3-carboxylic acid tert-butyl ester (4.35 g, 0.019 mol; see WO 01/28992), and the resultant mixture was then stirred at 50-55° C. overnight. After completion of the reaction (as determined by TLC), the mixture was filtered and concentrated. The crude product was further purified by column chromatography (silica gel: 60-120 mesh, eluent: chloroform-methanol, 99:1). Yield: 4.2 g (46%).
WORKUP
后处理
- customAfter completion of the reaction (as determined by TLC)
- filtrationthe mixture was filtered
- concentrationconcentrated
- customThe crude product was further purified by column chromatography (silica gel: 60-120 mesh, eluent: chloroform-methanol, 99:1)