反应详情

温度

105 °C

A solution of 50 ml of toluene and 7.9 g of dibenzylamine are added dropwise with stirring at 50-60° C. in the course of 10 min. to 5.2 g of 5-bromobenzofuran-2-carbonyl chloride in 100 ml of toluene. A colourless solid is obtained. After dropwise addition is complete, the mixture is additionally stirred at 100-110° C. for a further 3 hours. After cooling to 10° C., the solid product (dibenzylammonium chloride) is filtered off with suction. The filtrate is then treated with a mixture of 150 ml of water and 10 g of sodium carbonate and thoroughly shaken. The organic phase is separated off, washed again with 100 ml of water, dried using sodium sulfate and filtered. The, filtrate is concentrated on a Rotavapor in vacuo to a residue (residue: 9.5 g). After recrystallization from 100 ml of methanol, 6.5 g of product (yield 77%) remain after isolation.

1. customA colourless solid is obtained
2. additionAfter dropwise addition
3. temperatureAfter cooling to 10° C.
4. filtrationthe solid product (dibenzylammonium chloride) is filtered off with suction
5. additionThe filtrate is then treated with a mixture of 150 ml of water and 10 g of sodium carbonate
6. stirringthoroughly shaken
7. customThe organic phase is separated off
8. washwashed again with 100 ml of water
9. customdried
10. filtrationfiltered
11. concentrationThe, filtrate is concentrated on a Rotavapor in vacuo to a residue (residue: 9.5 g)