HRID2075593

反应详情

EQUATION

反应方程式

HRID 2075593 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To 5-tert-butyl-2-p-tolyl-2H-pyrazole-3-carboxylic acid ethyl ester (0.5 g, 1.75 mmol) in a 40 mL scintillation vial was added 2 mL THF and 2 mL 1N LiOH. The reaction was heated at 50° C. for 1 hr after which the reaction mixture was concentrated under vacuum and the crude residue was diluted with 5 mL 1N HCl. The reaction slurry was then extracted with DCM (3×25 mL) and the combined organic layers were washed with brine (10 mL) and dried over MgSO4. The resulting solution was concentrated under vacuum to yield the desired product (0.432 g, 96%) in >95% purity. The isolated material was used without further purification.

WORKUP

后处理

  1. concentrationwas concentrated under vacuum
  2. additionthe crude residue was diluted with 5 mL 1N HCl
  3. extractionThe reaction slurry was then extracted with DCM (3×25 mL)
  4. washthe combined organic layers were washed with brine (10 mL)
  5. dry with materialdried over MgSO4
  6. concentrationThe resulting solution was concentrated under vacuum