HRID76019

反应详情

EQUATION

反应方程式

HRID 76019 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ice cold solution of 1-[2-(4-tert-butyl-benzenesulfonylamino)-5-chloro-phenyl]-1H-pyrazole-4-carboxylic acid ethyl ester (synthesized according to general procedure D, 220 mg, 0.47 mmol) in THF (5 mL) was added LiAlH4 (1.0 mL, 2.4 M solution in THF) dropwise and the resultant reaction mixture was stirred for one hour at room temperature. Saturated Na2SO4 solution (3 mL) was subsequently added slowly at 0° C. and the precipitated solid was filtered through celite and washed thoroughly with EtOAc (100 mL). The filtrate was dried over Na2SO4, concentrated in vacuo, and purified by automated flash chromatography to afford the title compound: MS (ES) M+H expected 420.1, found 420.1.

WORKUP

后处理

  1. customthe resultant reaction mixture
  2. filtrationthe precipitated solid was filtered through celite
  3. washwashed thoroughly with EtOAc (100 mL)
  4. dry with materialThe filtrate was dried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. custompurified by automated flash chromatography