HRID2351966
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 3.1 g. portion of 3-(1-methylhexylaminomethyl)pyridine was dissolved in dichloromethane with stirring, and to it were added 2.1 g. of potassium carbonate and 1.16 ml. of methanesulfonyl chloride with cooling in an ice bath. The mixture was stirred at ambient temperature for 4 days. The reaction mixture was then extracted twice with 15 ml. portions of water, and the organic layer was dried over magnesium sulfate, filtered and evaporated under vacuum. The residue was dissolved in ethyl acetate and purified by chromatography over silica gel in ethyl acetate. The product-containing fractions were combined to obtain 1.7 g. of the desired product. Elemental analysis:
WORKUP
后处理
- additionto it were added 2.1 g
- stirringThe mixture was stirred at ambient temperature for 4 days
- extractionThe reaction mixture was then extracted twice with 15 ml
- dry with materialportions of water, and the organic layer was dried over magnesium sulfate
- filtrationfiltered
- customevaporated under vacuum
- dissolutionThe residue was dissolved in ethyl acetate
- custompurified by chromatography over silica gel in ethyl acetate
- customto obtain 1.7 g