HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 9864893, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 11266768 | HCID 11266768 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 9864893 | HCID 9864893 | 52% |
Reaction Steps
To a solution of 3-[6-methyl-3-(3-phenylpropyl)-3-azabicyclo[3.1.0]hex-6-yl]phenylamine (Preparation 8, 28 mg, 0.09 mmol) in dichloromethane (2 ml), at 0° C. under nitrogen was added pyridine (20 μl, 0.24 mmol) and then methanesulfonylchloride (25 μl, 37 mg , 0.32 mmol) over 5 minutes. The mixture was allowed to warm to room temperature and was then stirred for 2 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 colourless oil (18 mg, 52%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06313312B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-77f71a8c3d524c6bb47296ad0ab34285 |
| Source note | uspto-grants-2001_11 |