HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 19369246, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 19369278 | HCID 19369278 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 19369246 | HCID 19369246 | — |
Reaction Steps
Example 296 B) To the hexahydro-7-[2-(2-piperidyl) ethyl]-1H-azepin-2-one product of Example 296 A (2-3 g, 10 mmol) in anhydrous pyridine (8 mL) and CH2Cl2 (4 mL) was added dropwise methanesulfonyl chloride (0.74 mL) in CH2Cl2 (2 mL). The contents were stirred overnight, concentrated in vacuo and partitioned between CH2Cl2 and water. The CH2Cl2 layer was dried over MgSO4 and concentrated in vacuo leaving an oil. The oil was purified by C18 reverse phase chromatography eluding with a CH3CN/H2O (0.05% TFA) gradient to give hexahydro-7-[2-(2-methylsulfonylpiperidyl)ethyl]-1H-azepin-2-one (1.5 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06011028 |
| Source dataset | uspto-grants-2000_01 |
| ORD ID | ord-9776bd081c454022b97d9f04b980afff |
| Source note | uspto-grants-2000_01 |