HRID2272954

反应详情

EQUATION

反应方程式

HRID 2272954 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A solution of 547 mg (1.61 mmol) 6-(4-tert-butyl-phenyl)-4-oxo-4,5-dihydro-pyrazolo[1,5-a]pyrazine-2-carboxylic acid ethyl ester in 10 ml 1,2-dimethoxyethane is treated with 5 ml 1 N aqueous NaOH solution. The resulting suspension is heated to 100° C. and the resulting solution is stirred at this temperature for 48 hours. The reaction mixture is cooled to room temperature and evaporated. The residue is triturated with water and the solids are filtered off and washed with water. The filtrate is acidified with 2 N HCl. The resulting precipitate is filtered off, washed with 2 N HCl and with water and dried under vacuum to give 6-(4-tert-butyl-phenyl)-4-oxo-4,5-dihydro-pyrazolo[1,5-a]pyrazine-2-carboxylic acid as colourless solid; HPLC/MS 2.03 (A), [M+H] 312.

WORKUP

后处理

  1. temperatureThe reaction mixture is cooled to room temperature
  2. customevaporated
  3. customThe residue is triturated with water
  4. filtrationthe solids are filtered off
  5. washwashed with water
  6. filtrationThe resulting precipitate is filtered off
  7. washwashed with 2 N HCl and with water
  8. customdried under vacuum