HRID51907

反应详情

EQUATION

反应方程式

HRID 51907 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

7-[(4′-Trifluoromethyl-biphenyl-2-carbonyl)-amino]-quinoline-3-carboxylic acid ethyl ester (10.28 g, 22.1 mmol) and lithium hydroxide monohydrate (1.86 g, 44.3 mmol) were added to 125 ml of a solution consisting of a 3:1:1 volume ratio of tetrahydrofuran, methanol, and water. After stirring for 3.5 h at ambient temperature, the mixture was concentrated under vacuum to yield an aqueous emulsion of a yellow oil. More water (100 ml) was added and with efficient stirring, the aqueous mixture was made acidic (pH 2) with a 1 N aqueous hydrochloric acid solution. Collection of the resulting solid by vacuum filtration, maintaining the flow of air overnight to dry the solid, and drying under vacuum afforded 9.0 g of the title compound as a yellow powder.

WORKUP

后处理

  1. concentrationthe mixture was concentrated under vacuum
  2. customto yield an aqueous emulsion of a yellow oil
  3. customCollection of the resulting solid
  4. filtrationby vacuum filtration
  5. temperaturemaintaining the flow of air overnight
  6. customto dry the solid
  7. customdrying under vacuum