反応 #716786

反応方程式

suspension

tert-butyl 4-((4′-chloro-4-(trifluoromethylsulfonyloxy)biphenyl-2-yl)methyl)piperazine-1-carboxylate

N,N-dimethylprop-2-yn-1-amine

triethylamine

tert-butyl ammonium iodide

→

title compound

tert-butyl 4-((4′-chloro-4-(3-(dimethylamino)prop-1-ynyl)biphenyl-2-yl)methyl)piperazine-1-carboxylate

溶媒

ethyl acetate

N,N-dimethylformamide

反応条件

後処理

1. 1
   洗浄The organic phase was washed with water, brine
2. 2
   乾燥dried over anhydrous sodium sulfate
3. 3
   ろ過filtered
4. 4
   濃縮concentrated
5. 5
   その他The crude material was purified by flash column purification with 0-3% methanol/dichloromethane

実験手順

A suspension of EXAMPLE 198B (800 mg), N,N-dimethylprop-2-yn-1-amine (373 mg), copper(I) iodide (57 mg), tetrakis(triphenylphosphine)palladium(O) (259 mg), triethylamine (757 mg) and tert-butyl ammonium iodide (829 mg) in anhydrous N,N-dimethylformamide (5 mL) was heated at 100° C. for 5 hours. The reaction mixture was cooled to room temperature and diluted with ethyl acetate. The organic phase was washed with water, brine, dried over anhydrous sodium sulfate, filtered, and concentrated. The crude material was purified by flash column purification with 0-3% methanol/dichloromethane to afford the title compound.

出典