HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 4-Methanesulphonamido-1-(4-phenyl-4-oxobutyl)piperidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 4-Amino-1-(4-phenyl-4-oxobutyl)piperidine | HCID 12608537 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-Methanesulphonamido-1-(4-phenyl-4-oxobutyl)piperidine | HCID 21426525 | — |
Reaction Steps
4-Amino-1-(4-phenyl-4-oxobutyl)piperidine (1.23 g. 0.005 m) was suspended in a solution of dichloromethane (10 mls) containing triethylamine (2 mls). Methanesulphonyl chloride (0.570 g, 0.005 m) in dichloromethane (5 mls) was added dropwise over 5 minutes and the reaction stirred overnight at room temperature. The solution was then washed with five aliquots of water and dried over magnesium sulphate. Evaporation yielded the free base in 90% purity. This was triturated in ethyl acetate and warmed. The mother liquor was decanted off and evaporated to yield the title compound m.pt 141.4° C. This was recrystallised from ethanolic HCl as the hydrochloride salt (0.510 g), m.pt 167.4° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04034098 |
| Source dataset | uspto-grants-1977_07 |
| ORD ID | ord-516f769c74dc4c6db94b5b6c9bfb32dc |
| Source note | uspto-grants-1977_07 |