反应详情

A mixture of 2-[3-bromo-(5-trifluoromethyl-pyridin-2-yloxy)-phenyl]-ethylamine (950 mg, 2.059 mmol) and copper(I)cyanide (239.78 mg, 2.677 mmol, 1.3 eq) were suspended in N-methylpyrrolidone (2.1 ml) was irradiated in microwave Biotage Initiator at 200° C. for 20 min. After cooling, water (20 ml) was added and extraction with EtOAc (3×15 ml) followed. Organic layers were combined, dried over Na2SO4/MgSO4, filtered off and evaporated in vacuo to give crude 5-(2-amino-ethyl)-2-(5-trifluoromethyl-pyridin-2-yloxy)-benzonitrile. Crude product was put on a previously conditioned SCX column (5 g). The column was washed with MeOH (2×10 ml) and then with 2N NH3/MeOH (2×10 ml) to retrieve the product 5-(2-amino-ethyl)-2-(5-trifluoromethyl-pyridin-2-yloxy)-benzonitrile (245 mg, 0.797 mmol, yield=38%, purity=91%). [M+H]+=308.23 1H NMR (300 MHz, CDCl3) δ/ppm 2.79 (br. s., 2H), 2.94-3.07 (m, 2H), 7.21 (br. s., 2H), 7.49 (d, J=8.9 Hz, 1H), 7.54 (br. s., 1H), 7.90-8.05 (m, 1H), 8.38 (br. s., 1H)

1. customwas irradiated in microwave Biotage Initiator at 200° C. for 20 min
2. temperatureAfter cooling
3. extractionextraction with EtOAc (3×15 ml)
4. dry with materialdried over Na2SO4/MgSO4
5. filtrationfiltered off
6. customevaporated in vacuo