反応 #676581

ord-9765130a361347f9ba1e22b136376228

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-(6-methylnicotinamido)benzyl]-1H-indazol-3-yl]acetate (258 mg, 0.60 mmol) was dissolved in tetrahydrofuran (20 mL), and in an ice bath, 10 mL aqueous solution dissolving lithium hydroxide monohydrate (76 mg, 1.81 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 230 mg, at a yield of 95.4%.

出典

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