HRID388260
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheated to reflux
- temperatureThe reaction mixture was then cooled
- customthe solvents removed under reduced pressure
- additionThe crude oil was diluted with EtOAc
- washwashed with H2O
- dry with materialthe organic phase dried over Na2SO4
- filtrationfiltered
- customthe solvents removed under reduced pressure
- customto yield a yellow oil which
- customwas purified by flash chromatography on silica gel