反応 #676578

反応方程式

hydrochloric acid

Ethyl 2-[1-[4-(4-cyanobenzamido)benzyl]-1H-indazol-3-yl]acetate

lithium hydroxide monohydrate

Water

→

solid

収率 60.9%

2-[1-[4-(4-cyanobenzamido)benzyl]-1H-indazol-3-yl]acetic acid

収率 60.9%

溶媒

tetrahydrofuran

—

aqueous solution

反応条件

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
6. 6
   その他the resulting solid was recrystallized from ethyl acetate

実験手順

Ethyl 2-[1-[4-(4-cyanobenzamido)benzyl]-1H-indazol-3-yl]acetate (121 mg, 0.276 mmol) was dissolved in tetrahydrofuran (20 mL), and in an ice bath 10 mL aqueous solution dissolving lithium hydroxide monohydrate (58 mg, 1.38 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, and the resulting solid was recrystallized from ethyl acetate to obtain a white solid 69 mg, at a yield of 60.9%.

出典