HRID434197

反应详情

EQUATION

反应方程式

HRID 434197 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

In 350 ml of methylene chloride was dissolved 74.4 g of 2-ethyl-2-bicyclo[2.2.1]heptyl 3-hydroxybutanoate (which was synthesized by reacting 2-ethyl-2-bicyclo[2.2.1]heptyl acetate with acetoaldehyde in the presence of lithium hexamethyldisilazide). Then 39.0 g of pyridine and a catalytic amount of 4-(N,N-dimethylamino)pyridine were added to the solution, which was stirred under ice cooling. To this reaction mixture below 10° C., 66.8 g of 2-norbornene-5-carboxylic chloride was added dropwise over one hour. After agitation was continued for 3 hours, the reaction solution was worked up in a conventional manner. The resulting oily substance was purified by silica gel column chromatography, obtaining 96.7 g of 2-(2-ethyl-2-bicyclo[2.2.1]-heptyloxycarbonyl)propyl 2-norbornene-5-carboxylate, designated Monomer 1. The yield was 84.9%.

WORKUP

后处理

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  2. customThe resulting oily substance was purified by silica gel column chromatography