反应详情

43.66 g (156.0 mmol) of TBAF was added to a solution of 46.50 g (142.0 mmol) of 2-[(tert-butyldimethylsilanyl)ethynyl]-5-(4-chlorophenyl)pyridine in 1 L of DCM at RT and the mixture was stirred for 2 hours. The organic phase was washed with water, dried over sodium sulfate, and evaporated down in vacuo. The residue was stirred with DIPE, and the precipitate was filtered off and washed with PE. Yield: 26.0 g (86% of theoretical); C13H8ClN (M=213.662); calc.: molpeak (M+H)+: 214/216 (Cl); found: molpeak (M+H)+: 214/216 (Cl); Rf value: 0.30 (silica gel, cyc/EtOAc 4:1).

1. washThe organic phase was washed with water
2. dry with materialdried over sodium sulfate
3. customevaporated down in vacuo
4. stirringThe residue was stirred with DIPE
5. filtrationthe precipitate was filtered off
6. washwashed with PE