HRID2266422

反应详情

EQUATION

反应方程式

HRID 2266422 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of [8-chloro-3-(4-chlorobenzyl)-2,4-dimethylquinolin-5-yloxy]acetic acid methyl ester (0.11 g), acetonitrile (2.0 mL) and 4.0 M aqueous lithium hydroxide solution (2.0 mL) was stirred at room temperature for 1 hour. The acetonitrile was removed under reduced pressure and the pH of the residue adjusted to 5 by the addition of saturated aqueous sodium dihydrogenphosphate solution. The resulting mixture was extracted with ethyl acetate and the combined extracts dried over magnesium sulfate and concentrated under reduced pressure. Purification of the residue by column chromatography on a flash NH2 cartridge, eluting with methanol and then 2.0 M ammonia in methanol, gave title compound, 0.10 g.

WORKUP

后处理

  1. customThe acetonitrile was removed under reduced pressure
  2. additionthe pH of the residue adjusted to 5 by the addition of saturated aqueous sodium dihydrogenphosphate solution
  3. extractionThe resulting mixture was extracted with ethyl acetate
  4. dry with materialthe combined extracts dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customPurification of the residue by column chromatography on a flash NH2 cartridge
  7. washeluting with methanol