反应详情

温度

85 °C

In 20 g of toluene was suspended 6.28 g of AlCl3 in a stream of argon, to which 20 g of DMF was then added dropwise at 26° C. before adding 10.0 g of compound (1a), followed by heat stirring at 85° C. for 1.5 hours. The reaction mixture was cooled, to which 5.89 g of 35% hydrochloric acid was then added dropwise before adding 17.0 g of water, followed by heat stirring at 75° 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 9.0 g of compound (2a) at a yield of 96%.

1. temperatureby heat
2. additionwas then added dropwise
3. temperatureby heat
4. stirringstirring at 75° 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.