反応 #62327

反応方程式

water

3-[(E)-2-(4-fluorophenyl)-vinyl]-4-[2-(tetrahydropyran-2-yloxy)-ethoxy]-1H-indazole-1,5-dicarboxylic acid 1-tert-butyl ester 5-ethyl ester

hydrochloric acid

→

title compound

収率 69.8%

3-[(E)-2-(4-Fluorophenyl)-vinyl]-4-(2-hydroxyethoxy)-1H-indazole-1,5-dicarboxylic acid 1-tert-butyl ester 5-ethyl ester

収率 69.8%

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   抽出extracted twice ethyl acetate
2. 2
   洗浄the resultant organic layer was washed once with saturated brine
3. 3
   乾燥dried over magnesium sulfate
4. 4
   その他The solvent was evaporated
5. 5
   その他the crude product was purified
6. 6
   その他separated by silica gel column chromatography

実験手順

To a solution of 147 mg of 3-[(E)-2-(4-fluorophenyl)-vinyl]-4-[2-(tetrahydropyran-2-yloxy)-ethoxy]-1H-indazole-1,5-dicarboxylic acid 1-tert-butyl ester 5-ethyl ester in 1.5 mL of tetrahydrofuran was added 1.5 mL of 2N hydrochloric acid, and stirred at room temperature for 19 hours. Thereafter, the reaction solution was added with water and extracted twice ethyl acetate, and the resultant organic layer was washed once with saturated brine, and dried over magnesium sulfate. The solvent was evaporated, and the crude product was purified and separated by silica gel column chromatography, to afford 87.1 mg of the title compound as a colorless oil.

出典