HRID867962

反应详情

EQUATION

反应方程式

HRID 867962 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-(1H-1,2,4-triazol-1-yl)-N-methyl-1-(2-naphthalenyl)ethanimine N-oxide (15.0 g, 0.056 mol) and trans-1-phenyl-1,3-butadiene (11.0 g, 0.084 mol) in 500 ml toluene is heated to 95°-105° C. for 48 hours, then cooled and evaporated to dryness. The resulting oil is decolorized with carbon and purified by flash chromatography on silica gel (eluent comprised of 90% ethyl acetate and 10% hexane by volume) giving two diastereomers. Isomer A (5.66 g) has a melting point of 80°-84° C. (ethyl acetate-pentane). Isomer B (1.64 g) has a melting point 157°-160° C.

WORKUP

后处理

  1. temperatureis heated to 95°-105° C. for 48 hours
  2. temperaturecooled
  3. customevaporated to dryness
  4. custompurified by flash chromatography on silica gel (eluent comprised of 90% ethyl acetate and 10% hexane by volume)
  5. customgiving two diastereomers