HRID602778

反应详情

EQUATION

反应方程式

HRID 602778 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

300 mg (2.54 mmol) of amino-hydroxyimino-acetic acid methyl ester and 428 mg (2.29 mmol, 0.9 eq) of phenylsulfanyl-acetyl chloride were stirred in 10 mL of THF at RT for 1 hour. The solvent was evaporated, the residue dissolved in dioxane, and the reaction mixture was heated at reflux over night in the presence of molecular sieves. Filtration, concentration under vacuum and column chromatography over silica gel with EtOAc/heptane 1:1 yielded 310 mg (49%) of 5-phenylsulfanylmethyl-[1,2,4]oxadiazole-3-carboxylic acid methyl ester as light yellow oil, MS: 268 (MNH4+).

WORKUP

后处理

  1. customThe solvent was evaporated
  2. dissolutionthe residue dissolved in dioxane
  3. temperaturethe reaction mixture was heated
  4. temperatureat reflux over night in the presence of molecular sieves
  5. filtrationFiltration, concentration under vacuum and column chromatography over silica gel with EtOAc/heptane 1:1