HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → N-[3-(3-{3-Phenylpropyl}-3-azabicyclo[3.1.0]hex-6-yl)phenyl]methanesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 3-[3-(3-Phenylpropyl)-3-azabicyclo[3.1.0]hex-6-yl]phenylamine | HCID 22141154 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-[3-(3-{3-Phenylpropyl}-3-azabicyclo[3.1.0]hex-6-yl)phenyl]methanesulfonamide | HCID 22141129 | 71.2% |
Reaction Steps
To a solution of 3-[3-(3-phenylpropyl)-3-azabicyclo[3.1.0]hex-6-yl]phenylamine (Preparation 25, 34 mg, 0.11 mmol) in dichloromethane (2 ml) at 0° C. under nitrogen was added pyridine (20 μl, 0.24 mmol) then methanesulfonylchloride (13 mg, 10 μl, 0.11 mmol). The mixture was allowed to warm to room temperature and was stirred for 1.5 hours. The mixture was concentrated in vacuo and the residue was purified by silica (5 g) column chromatography eluting with 80:20:1 ethyl acetate:hexane:ammonia solution (0.880). Product-containing fractions were combined and concentrated in vacuo to give the title compound as a pale yellow oil (29 mg, 71%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06313312B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-acd589fc4b204c6db630fe79e1d9c665 |
| Source note | uspto-grants-2001_11 |