HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 69524564, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 69525013 | HCID 69525013 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69524564 | HCID 69524564 | 25% |
Reaction Steps
To the amine from Step (b) (0.116 g, 0.3 mmol) in dry dichloromethane (5 ml) was added pyridine (0.060 ml, 0.75 mmol), followed by methanesulfonyl chloride (0.035 ml, 0.45 mmol), and the mixture was stirred at room temperature for 48 hours. After dilution with water (20 ml) and extraction with ethyl acetate (3×20 ml), the combined organic fractions were washed with brine, dried (MgSO4 and evaporated under reduced pressure. The residue was purified by flash chromatography eluting with 10% to 30% ethyl acetate in iso-hexane to give as a mixture of diastereoisomers the title compound as a colourless oil (35 mg, 25%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07161006B2 |
| Source dataset | uspto-grants-2007_01 |
| ORD ID | ord-31261fc2bba44c34bd92ac7f7de3b40c |
| Source note | uspto-grants-2007_01 |