反応 #1005945

反応方程式

sodium carbonate

t-butyl {4-[3-(3,5-dichlorophenyl)-3-(trifluoromethyl)-pyrrolidin-1-yl]-2-(trifluoromethyl)benzyl}carbamate

hydrochloric acid

ethanol

→

title compound

収率 105.6%

1-{4-[3-(3,5-dichlorophenyl)-3-(trifluoromethyl)-pyrrolidin-1-yl]-2-(trifluoromethyl)phenyl}methanamine

収率 105.6%

溶媒

ethyl acetate

water

反応条件

後処理

1. 1
   workup.ADDITIONthe reaction solution was diluted
2. 2
   抽出After the extraction
3. 3
   洗浄the organic layer was washed with saturated brine
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   その他The solvent was evaporated off under reduced pressure

実験手順

A mixture comprising t-butyl {4-[3-(3,5-dichlorophenyl)-3-(trifluoromethyl)-pyrrolidin-1-yl]-2-(trifluoromethyl)benzyl}carbamate (6.0 g), concentrated hydrochloric acid (20 mL) and ethanol (100 mL) was stirred at 50° C. for three hours. After cooling the mixture to room temperature, the reaction solution was diluted by adding water (150 mL) and ethyl acetate (150 mL). By adding sodium carbonate in small portions, the solution was neutralized. After the extraction using ethyl acetate, the organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated off under reduced pressure to obtain the title compound (5.2 g).

出典