反应详情

温度

10 °C

HCl/EtOH ˜10% (35.1 ml, 115 mmol) was set into the reaction flask under nitrogen atmosphere. 2-Chloro-4-(1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)-benzonitrile (12 g, 46.2 mmol) was added. The mixture was cooled to 10° C. and agitated for 2 h. Temperature was set to 0° C. and the mixture was stirred additional 2 hours. The precipitation was filtered, washed with ethanol and dried under vacuum overnight to obtain 9.24 g of the title compound. 1H-NMR (400 MHz, DMSO-d6): δ 6.99 (d, 3H), 7.86 (d, 1H), 7.96-8.02 (m, 2H), 8.14-8.17 (m, 1H).

1. customwas set to 0° C.
2. stirringthe mixture was stirred additional 2 hours
3. customThe precipitation
4. filtrationwas filtered
5. washwashed with ethanol
6. customdried under vacuum overnight