HRID399845

反应详情

EQUATION

反应方程式

HRID 399845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The mixture of 3-(5-amino-4-carboxypyrazol-1-yl)benzoic acid (19.4 g) in diglyme (200 ml) was heated under reflux for 6 hours. To the mixture was added a mixture of ethyl acetate and water, and adjusted to pH 9 with 20% aqueous potassium carbonate solution. The separated aqueous layer was adjusted to pH 3.5 with 6N-hydrochloric acid and the mixture was extracted with a solution of ethyl acetate and tetrahydrofuran. The extract layer was washed with brine, dried over magnesium sulfate and evaporated in vacuo to give 3-(5-aminopyrazol-1-yl)benzoic acid (7.59 g).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 6 hours
  3. additionTo the mixture was added
  4. extractionthe mixture was extracted with a solution of ethyl acetate and tetrahydrofuran
  5. washThe extract layer was washed with brine
  6. dry with materialdried over magnesium sulfate
  7. customevaporated in vacuo