反应详情

温度

160 °C

4-Bromo-3-Chloro-5-fluoroaniline (980 mmol, 220 g), copper(I)cyanide (980 mmol, 88 g) and NMP (1000 ml) were added into the reaction flask, heated up to 160° C. and stirred for 3 h to complete the reaction. The reaction mixture was cooled to RT. Water and 25% ammonia solution was added keeping the mixture at RT. The mixture was stirred overnight and the formed precipitate was separated by filtration and flushed with water. The filtered precipitate was dried under vacuum to give 117.7 g of the title compound. 1H-NMR (400 MHz, DMSO-d6): δ 6.41-6.47 (m, 1H), 6.58-6.62 (m, 1H), 6.86 (bs, 2H).

1. customthe reaction
2. temperatureThe reaction mixture was cooled to RT
3. customat RT
4. stirringThe mixture was stirred overnight
5. customthe formed precipitate was separated by filtration
6. customflushed with water
7. customThe filtered precipitate was dried under vacuum