反应详情

温度

0 °C

A mixture of methyl indole-3-carboxylate and dichloromethane is cooled to 0° C. 1,4-dimethylpiperazine (0.55 eq.) and N-chlorosuccinimide (1.1 eq) are added and the mixture left to stir for two hours to give a slurry containing the compound of formula (C) above. The resulting slurry is added to a solution of 3-chloropropanol (1.1 eq) and trichloroacetic acid (0.12 eq) in dichloromethane, maintaining the temperature below 0° C. The reaction mixture is left to stir for half an hour, then washed with 10% aqueous sodium carbonate, 0.5 M hydrochloric acid and water. The organic solution is dried over sodium sulphate, filtered and the solvent evaporated. Toluene is added and the mixture stirred at 0-5° C. for one hour. The product is then filtered, washed with toluene and dried to give the title product in 83% yield.

1. waitthe mixture left
2. customto give a slurry
3. temperaturemaintaining the temperature below 0° C
4. waitThe reaction mixture is left
5. stirringto stir for half an hour
6. washwashed with 10% aqueous sodium carbonate, 0.5 M hydrochloric acid and water
7. dry with materialThe organic solution is dried over sodium sulphate
8. filtrationfiltered
9. customthe solvent evaporated
10. additionToluene is added
11. stirringthe mixture stirred at 0-5° C. for one hour
12. filtrationThe product is then filtered
13. washwashed with toluene
14. customdried