HRID388260

反应详情

EQUATION

反应方程式

HRID 388260 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of methyl 2-(methylthio)-2-phenylacetate (0.300 g, 1 equiv) in anhydrous EtOH (5 mL) was added hydrazine hydrate (0.15 mL, 2 equiv) and heated to reflux. Stirring was then continued for 18 hours. The reaction mixture was then cooled and the solvents removed under reduced pressure. The crude oil was diluted with EtOAc and washed with H2O and the organic phase dried over Na2SO4, filtered, and the solvents removed under reduced pressure to yield a yellow oil which was purified by flash chromatography on silica gel using ethyl acetate and hexanes. The purified product was a white solid (193 mg, 66%).

WORKUP

后处理

  1. temperatureheated to reflux
  2. temperatureThe reaction mixture was then cooled
  3. customthe solvents removed under reduced pressure
  4. additionThe crude oil was diluted with EtOAc
  5. washwashed with H2O
  6. dry with materialthe organic phase dried over Na2SO4
  7. filtrationfiltered
  8. customthe solvents removed under reduced pressure
  9. customto yield a yellow oil which
  10. customwas purified by flash chromatography on silica gel