反应详情

To a stirred mixture of 60.5 parts of α-methyl-1,4-bis(phenylmethyl)-2-piperazinemethanol and 180 parts of N,N-dimethylformamide were added portionwise 29.8 parts of a sodium hydride dispersion 50% at a temperature below 35° C. under nitrogen atmosphere. The mixture was allowed to cool and stirred for 3 hours at room temperature. After cooling to 10° C., there were added dropwise 9.4 parts of iodomethane at about 20° C. Upon completion, stirring was continued for 2 hours at room temperature. The reaction mixture was poured onto water and the product was extracted twice with 1,1'-oxybisethane. The combined extracts were washed with water, dried, filtered and evaporated, yielding 45.2 parts (71.5%) of 2-(1-methoxyethyl)-1,4-bis(phenylmethyl)piperazine as a residue (intermediate 28).

1. temperatureto cool
2. temperatureAfter cooling to 10° C.
3. stirringUpon completion, stirring
4. waitwas continued for 2 hours at room temperature
5. additionThe reaction mixture was poured onto water
6. extractionthe product was extracted twice with 1,1'-oxybisethane
7. washThe combined extracts were washed with water
8. customdried
9. filtrationfiltered
10. customevaporated