HRID2270233

反应详情

EQUATION

反应方程式

HRID 2270233 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-chloro-2-cyclopropylamino-5-fluoro-benzoic acid ethyl ester (Example B-3, 4.10 g, 15.9 mmol) in THF (100 mL) was reacted with an aqueous solution of 1.0 N LiOH (45 mL, 45 mmol) and methanol (40 mL) and allowed to stir overnight. The mixture was then concentrated to one-third volume and acidified with 1.0 N HCl. The mixture was extracted with ethyl acetate. the organic layers combined, dried with sodium sulfate, and concentrated to provide 3.0 g of the title compound as an oil.

WORKUP

后处理

  1. concentrationThe mixture was then concentrated to one-third volume
  2. extractionThe mixture was extracted with ethyl acetate
  3. dry with materialdried with sodium sulfate
  4. concentrationconcentrated