反应详情

187 g (2 mols) N,N-dimethylmethyleneammonium chloride are suspended under an inert gas (nitrogen or argon) in 28 liters anhydrous acetonitrile. The stirred suspension is mixed with 159 g (1 mol) pulverized and dried 2-acetylindole, heated to the boil and, while stirring continuously, uniformly cooled over the course of 7 hours to 25° C. It is stirred overnight at 20°-25° C. The acetonitrile is substantially distilled off under vacuum and the remaining residue taken up in 20 liters of water and adjusted to pH 9-10 with concentrated ammonium hydroxide solution. This solution is stirred up three times with, in each case, 5 liters of dichloromethane. The organic phases are combined and washed with 5 liters of water. The organic phase is dried by the addition of anhydrous sodium sulphate, filtered and mixed with 5 liters tert-butyl methyl ether. The dichloromethane is substantially distilled off, the crystallization of the product thereby already commencing. This is completed by leaving to stand overnight at +4° C. The product is filtered off with suction, washed with n-hexane and dried under a vacuum. Yield: 141.7 g (65.6% of theory).

1. additionThe stirred suspension is mixed with 159 g (1 mol)
2. temperatureuniformly cooled over the course of 7 hours to 25° C
3. stirringIt is stirred overnight at 20°-25° C
4. distillationThe acetonitrile is substantially distilled off under vacuum
5. stirringThis solution is stirred up three times with, in each case, 5 liters of dichloromethane
6. washwashed with 5 liters of water
7. dry with materialThe organic phase is dried by the addition of anhydrous sodium sulphate
8. filtrationfiltered
9. additionmixed with 5 liters tert-butyl methyl ether
10. distillationThe dichloromethane is substantially distilled off
11. customthe crystallization of the product
12. customby leaving
13. filtrationThe product is filtered off with suction
14. washwashed with n-hexane
15. customdried under a vacuum