反応 #8493

反応方程式

HCl

2-[2-(4-fluorophenyl)ethyl]-5-fluorobenzonitrile

NaOH

H2O

→

cream-colored solid

収率 88.4%

2-[2-(4-Fluorophenyl)ethyl]-5-fluorobenzoic acid

収率 88.4%

溶媒

ethylene glycol

反応条件

後処理

1. 1
   温度to cool
2. 2
   その他The cloudy mixture precipitated the desired product as a cream-colored solid
3. 3
   洗浄This material was washed with H2O (3×20 mL)
4. 4
   その他dried under vacuum (18 h, 25° C., 0.1 mm Hg)

実験手順

A mixture of 2-[2-(4-fluorophenyl)ethyl]-5-fluorobenzonitrile (2.12 g, 8.72 mmol, 1 equiv) and aq. NaOH (10N; 3.9 mL, 39.3 mmol, 4.5 equiv) in ethylene glycol (25 mL) was heated at 190° C. for 24 h. After allowing the mixture to cool, H2O (100 mL) was added followed by 12N HCl (8 mL). The cloudy mixture precipitated the desired product as a cream-colored solid. This material was washed with H2O (3×20 mL) and dried under vacuum (18 h, 25° C., 0.1 mm Hg) to provide 2.02 g (88.4%) of a cream-colored solid.

出典