反应详情

温度

60 °C

A suspension of crude 3-chloro-1H-indol-1-amine (65.5 g) and 4-chloropyridine hydrochloride (45 g) in 1-methyl-2-pyrrolidinone (250 ml) was stirred at 60° C. for eight hours. The cooled reaction mixture was quenched into 5% aqueous sodium hydroxide, extracted into toluene, dried and concentrated to give an oil. A portion of this oil was dissolved in ethyl acetate. Salicylic acid (1.2 eq) was added to precipitate the salt. The solid was collected at room temperature and dried. This solid was recrystallized with a charcoal treatment from methanol and oven dried (75° C., house vacuum) overnight to yield 10.9 g of the title compound as a solid, m.p. 185°-186° C. (dec.).

1. customThe cooled reaction mixture
2. customwas quenched into 5% aqueous sodium hydroxide
3. extractionextracted into toluene
4. customdried
5. concentrationconcentrated
6. customto give an oil
7. customto precipitate the salt
8. customThe solid was collected at room temperature
9. customdried
10. customThis solid was recrystallized with a charcoal treatment from methanol and oven
11. customdried (75° C., house vacuum) overnight