反应详情

27.0 g (1.11 mole) of magnesium turnings were stirred in 150 ml tetrahydrofuran and 207.6 g (1.11 mole) 1-bromo-3-methoxy-benzene, dissolved in 400 ml tetrahydrofuran, were added drop-wise. The mixture was heated for one hour under reflux and was subsequently cooled to a temperature between 5° C. and 10° C. 128.30 g (0.89 mole) (RS)-1-dimethylamino-2-methyl-pentan-3-one, dissolved in 400 ml tetrahydrofuran, were added drop-wise at this temperature. The reaction mixture was allowed to stand and was subsequently cooled again to a temperature between 5° C. and 10° C. After adding 300 ml of 20 weight % ammonium chloride solution, the mixture was diluted with 400 ml ether. After phase separation the batch was extracted twice with ether, dried over sodium sulphate and the solvent was removed by distillation. The residue obtained was taken up in 3.2 l 2-butanone and treated with 120.60 g (1.11 mole) trimethylchlorosilane and 20 ml water. 121.5 g of hydrochloride (2) (38% theoretical) with a melting point of 198°-199° C. were obtained. 2nd step:

1. additionwere added drop-wise
2. temperatureThe mixture was heated for one hour
3. temperatureunder reflux
4. temperaturewas subsequently cooled to a temperature between 5° C. and 10° C
5. additionwere added drop-wise at this temperature
6. temperaturewas subsequently cooled again to a temperature between 5° C. and 10° C
7. customAfter phase separation the batch
8. extractionwas extracted twice with ether
9. dry with materialdried over sodium sulphate
10. customthe solvent was removed by distillation
11. customThe residue obtained