反应 #163172

ord-bf41954589e448d88ca93ad18fa4c129

反应条件

温度
80°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The vial was sealed
  2. 2
    萃取The mixture was extracted with ethyl acetate (2×10 mL)
  3. 3
    浓缩the combined organics were concentrated in vacuo
  4. 4
    其他The resultant residue was purified via preparative HPLC

实验过程

A 25 mL scintillation vial was charged with 1-[3-(4-tert-butyl-benzenesulfonylamino)-5-chloro-pyridin-2-yl]-1H-pyrazole-4-carboxylic acid ethyl ester (synthesized according to general procedure D, 93 mg, 0.2 mmol), NaOH (2 mL, 1.0 M solution in water), and THF (3 mL). The vial was sealed and stirred at 80° C. for 16 hours. The reaction solution was subsequently neutralized to pH=5 with glacial acetic acid. The mixture was extracted with ethyl acetate (2×10 mL) and the combined organics were concentrated in vacuo. The resultant residue was purified via preparative HPLC to afford 1-[3-(4-tert-butyl-benzenesulfonylamino)-5-chloro-pyridin-2-yl]-1H-pyrazole-4-carboxylic acid as a white powder: MS (ES) M+H expected 435.1, found 435.0.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08835468B2uspto-grants-2014_09