HRID1078529

反应详情

EQUATION

反应方程式

HRID 1078529 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (S)-N-[[3-[3-fluoro-4-(1-piperazinyl)phenyl]-2-oxo-5-oxazolidinyl]methyl]acetamide (0.200 g, 0.595 mmol), 3-chloro-1-propanol (299 μL, 3.57 mmol) and potassium carbonate (0.493 g, 3.57 mmol) in acetonitrile (12 mL) was heated to reflux for 7 h. The reaction mixture was cooled to ambient temperature and concentrated in vacuo. The crude material was dissolved in 10% methanol/chloroform and absorbed onto silica gel (2 g). Chromatography of this material over silica gel (10 g), eluting with 1%, 3%, and then 6% methanol/chloroform, afforded, after concentration of appropriate fractions, 0.096 g (41%) of the title compound as a white solid with mp 154°-155.5° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 7 h
  3. concentrationconcentrated in vacuo
  4. dissolutionThe crude material was dissolved in 10% methanol/chloroform
  5. customabsorbed onto silica gel (2 g)
  6. washChromatography of this material over silica gel (10 g), eluting with 1%, 3%
  7. custom6% methanol/chloroform, afforded