HRID1613939

反应详情

EQUATION

反应方程式

HRID 1613939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 135 mg (0.978 mmols) of potassium carbonate in 1 ml of water was added to a solution of 349 mg (0.978 mmols) of 2-(1-hydroxy-2-nonynyl)-3-methyl-4-acetoxy-6-fluoroquinoline, 20 ml of methanol and 2 ml of water and stirred at room temperature for 10 minutes. After neutralization with 1N hydrochloric acid, the solvent was distilled off under reduced pressure, followed by addition of 20 ml of chloroform to the resultant residue, washing with water and drying with sodium sulfate. The solvent was distilled off under reduced pressure, followed by purification by silica gel column chromatography (Wako gel C-200) (solvent: n-hexane : ethyl acetate=1:1) to obtain 183 mg (yield 59 %) of 2-(1-hydroxy-2-nonynyl)-3-methyl-6-fluoro-4-quinolone.

WORKUP

后处理

  1. distillationAfter neutralization with 1N hydrochloric acid, the solvent was distilled off under reduced pressure
  2. additionfollowed by addition of 20 ml of chloroform to the resultant residue
  3. washwashing with water
  4. dry with materialdrying with sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customfollowed by purification by silica gel column chromatography (Wako gel C-200) (solvent: n-hexane : ethyl acetate=1:1)