HRID402373

反应详情

EQUATION

反应方程式

HRID 402373 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of pyridin-2-yl-propynoic acid ethyl ester (1.25 g, 7.14 mmol) in benzene (22 mL) was added azidomethyl-trimethyl-silane (1.11 g, 8.56 mmol) and the reaction mixture was refluxed under nitrogen for 72 h. The mixture was then evaporated and purification by chromatography [silica, 0 to 50% ethyl acetate in heptane then HPLC (Chiralpak AD, ethanol in heptane)] afforded the title compound (477 mg, 23%) as a yellow oil. MS: m/e=305.2 [M+H]+.

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed under nitrogen for 72 h
  2. customThe mixture was then evaporated
  3. custompurification by chromatography [silica, 0 to 50% ethyl acetate in heptane