تفاعل #676581

ord-9765130a361347f9ba1e22b136376228

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-(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%.

المصدر

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