反応 #676582

ord-c8ff4b5f52824ffc99a18504fab3e8f2

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    その他It was reacted at room temperature for 3 h
  3. 3
    その他A solid precipitated
  4. 4
    ろ過which was filtered
  5. 5
    その他dried

実験手順

Ethyl 2-[1-[4-(1-methyl-1H-pyrazol-4-carboxamido)benzyl]-1H-indazol-3-yl]acetate (279 mg, 0.67 mmol) was dissolved in tetrahydrofuran (20 mL), and in an ice bath, 10 mL aqueous solution dissolving lithium hydroxide monohydrate (84 mg, 2.0 mmol) was added. It was reacted at room temperature for 3 h, and the reaction was monitored to be complete by TLC. Water was added into the system, and adjusted to pH≈3-4 with diluted hydrochloric acid. A solid precipitated, which was filtered and dried to obtain a white solid 246 mg, at a yield of 94.5%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09233098B2uspto-grants-2016_01