反应详情

温度

100 °C

In 11 mL of dimethylformamide (DMF) were suspended 2.12 g of compound (1a), 4.82 g of AlCl3.6H2O, and 2.06 g of NaBr in a stream of argon, which was then heat stirred at 100° C. for 5 hours. The reaction mixture was allowed to stand to cool, to which 10.4 g of 35% hydrochloric acid was then added dropwise before adding 11 mL of water, followed by heat stirring at 70° C. for one hour. The precipitated crystal was collected by filtration and washed with water. The resultant crystal was dried under reduced pressure at 60° C. to provide 1.45 g of compound (2a) at a yield of 73%.

1. temperaturewas then heat
2. additionwas then added dropwise
3. temperatureby heat
4. stirringstirring at 70° C. for one hour
5. filtrationThe precipitated crystal was collected by filtration
6. washwashed with water
7. customThe resultant crystal was dried under reduced pressure at 60° C.