反应详情

A 6 g portion of 1,4-bis(phenylmethyl)-2-piperazinemethanol was dissolved in 90 ml of dichloromethane together with 4.26 ml of triethylamine and then cooled to 0°-5° C. A 2.04 ml portion of methanesulfonyl chloride was added and the mixture was allowed to warm to room temperature over 2 hours. The mixture was washed with ice cold sodium bicarbonate solution, followed twice with ice water, dried, filtered and evaporated. The residue was dissolved in dimethylformamide and added to a solution of 2.07 g of sodium phenol and 1.02 g of 50% sodium hydride in 30 ml of dimethylformamide under argon. This mixture was stirred for 48 hours, water was added and the mixture extracted twice with ether. The extracts were combined, washed with water, dried, filtered and evaporated, giving a gum which was crystallized from methanol with refrigeration, giving 4.1 g of 3-phenoxymethyl-1,4-bis(phenylmethyl)piperazine.

1. temperaturecooled to 0°-5° C
2. washThe mixture was washed with ice cold sodium bicarbonate solution
3. customdried
4. filtrationfiltered
5. customevaporated
6. dissolutionThe residue was dissolved in dimethylformamide
7. additionadded to a solution of 2.07 g of sodium phenol and 1.02 g of 50% sodium hydride in 30 ml of dimethylformamide under argon
8. additionwater was added
9. extractionthe mixture extracted twice with ether
10. washwashed with water
11. customdried
12. filtrationfiltered
13. customevaporated
14. customgiving a gum which
15. customwas crystallized from methanol with refrigeration