反应详情

温度

-40 °C

A solution of 2.19 g (0.00991 mol) of 1-methyl-3-(4-methylphenyl)-1H-indole and 3.24 mL (0.0218 mol) of TMEDA in 30 mL of ether was treated with 13.6 mL (0.0218 mol) of 1.6M BuLi in hexane under stirring at −40° C. Then the reaction mixture was allowed to warm up to r.t. and stirred for 4 h. The reaction mixture was cooled to −60° C. and treated with 1.16 g (0.00991 mol) ethyl N,N-dimethylcarbamate in 5 mL of ether. Then the reaction mixture was allowed to warm up to r.t. and was stirred overnight. Resulting mixture was treated with 50 mL of 10% aqueous NH4Cl. The violet precipitate was separated, washed twice with water and dried. Yield 1.04 g (42%).

1. temperatureto warm up to r.t.
2. stirringstirred for 4 h
3. temperatureThe reaction mixture was cooled to −60° C.
4. temperatureto warm up to r.t.
5. stirringwas stirred overnight
6. customResulting mixture
7. customThe violet precipitate was separated
8. washwashed twice with water
9. customdried