HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 68866370, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 57701104 | HCID 57701104 | — |
| Reactant | HCID 68865856 | HCID 68865856 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 68866370 | HCID 68866370 | 38% |
Reaction Steps
N-{5-[3-(3-Chloro-phenoxy)-4-methoxy-benzyl]-pyridin-2-yl}-methanesulfonamide HCl salt, P-09. To a 25 mL vial which contained 5-[3-(3-chloro-phenoxy)-4-methoxy-benzyl]-pyridin-2-ylamine P-05 (170 mg, 0.5 mmol) in pyridine (8 mL) was added methanesulfonyl chloride (144 mg, 1.3 mmol) at rt. The mixture was stirred at rt for 24 h. The mixture was poured into 50 mL ice-water and extracted with ethyl acetate, washed with water 1 N HCl, brine, and dried over Na2SO4. After it was concentrated in vacuo, the residue was purified by chromatography on silica gel with ethyl acetate/hexane as eluent to yield 80 mg (38% yield) of the desired product, P-09, using 2N HCl in ether was to convert into its HCl salt 50 mg (60% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08877816B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-8ade492876ec449b9145d1856c9a36d9 |
| Source note | uspto-grants-2014_11 |