反应详情

To 7.10 g of phenylmagnesium bromide (32% THF solution) was added dropwise a solution of 953 mg of 2-amino-3-chlorobenzonitrile in THF (7 ml) at room temperature, followed by heating under reflux for 30 minutes. To the resulting reaction product was added dropwise 885 mg of methyl chlorocarbonate under ice cooling, followed by heating under reflux for 40 minutes. The resulting reaction solution was cooled and poured into 40 ml of 2N-hydrochloric acid, and 8 g of sodium bicarbonate and 20 ml of MTBE were added thereto, followed by stirring. Then, precipitated crystals were collected by filtration to obtain 1.30 g of the titled compound. 1H NMR (DMSO-d6): 7.24(1H, t, J=8.0 Hz), 7.57-7.70 (6H, m), 7.90-7.93 (1H, m), 11.45 (1H,br. s).

1. temperatureby heating
2. temperatureunder reflux for 30 minutes
3. customTo the resulting reaction product
4. temperatureby heating
5. temperatureunder reflux for 40 minutes
6. customThe resulting reaction solution
7. temperaturewas cooled
8. additionwere added
9. customThen, precipitated crystals
10. filtrationwere collected by filtration