تفاعل #676582

ord-c8ff4b5f52824ffc99a18504fab3e8f2

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    أخرىIt was reacted at room temperature for 3 h
  3. 3
    أخرىA solid precipitated
  4. 4
    ترشيحwhich was filtered
  5. 5
    أخرىdried

الإجراء التجريبي

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%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09233098B2uspto-grants-2016_01