HRID2351966

反应详情

EQUATION

反应方程式

HRID 2351966 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionto it were added 2.1 g
  2. stirringThe mixture was stirred at ambient temperature for 4 days
  3. extractionThe reaction mixture was then extracted twice with 15 ml
  4. dry with materialportions of water, and the organic layer was dried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated under vacuum
  7. dissolutionThe residue was dissolved in ethyl acetate
  8. custompurified by chromatography over silica gel in ethyl acetate
  9. customto obtain 1.7 g