反应详情

To a solution of 8-ethyl-thienyl[3',4':6,5]dipyrido[2,3-b:3',2'-f]azepine (0.025 g) in tetrahydrofuran (2 mL) cooled to -78° C. was added lithium diisopropylamide (1.5M in cyclohexane, 0.1 mL). After 10 minutes, iodomethane (2 drops) was added, and the mixture was allowed to warm to room temperature. The mixture was diluted with ethyl acetate, washed with water, dried, filtered and evaporated. The residue was dissolved in tetrahydrofuran (2 mL) cooled to -78° C., and lithium diisopropylamide (1.5M in cyclohexane, 0.1 mL) was added. After 10 minutes, iodomethane (0.05 mL) was added, and the mixture was allowed to warm to room temperature. The mixture was diluted with ethyl acetate, washed with water, dried, filtered and evaporated. The residue was fractionated by HPLC to give 8-ethyl-1-methyl-thienyl[3',4':6,5]dipyrido[2,3-b:3',2'-f]azepine (0.010 g) mp 106-108° C. and 8-ethyl-1,3-dimethyl-thienyl[3',4':6,5]dipyrido[2,3-b:3',2'-f]azepine (0.003 g) mp 176-178° C.

1. washwashed with water
2. customdried
3. filtrationfiltered
4. customevaporated
5. dissolutionThe residue was dissolved in tetrahydrofuran (2 mL)
6. temperaturecooled to -78° C.
7. additionlithium diisopropylamide (1.5M in cyclohexane, 0.1 mL) was added
8. waitAfter 10 minutes
9. additioniodomethane (0.05 mL) was added
10. temperatureto warm to room temperature
11. additionThe mixture was diluted with ethyl acetate
12. washwashed with water
13. customdried
14. filtrationfiltered
15. customevaporated