HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 68511837, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 59467880 | HCID 59467880 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68511837 | HCID 68511837 | 60% |
Reaction Steps
To a 0° C. solution of compound 50 (160 g, 0.45 mmol) in dry CH2Cl2 (5 mL) was added methanesulfonyl chloride (70 μL, 0.90 mmol)) followed by dropwise addition of pyridine (100 μL, 1.40 mmol). The reaction was stirred overnight under N2. The reaction mixture was diluted with CH2Cl2 (40 mL), washed with 1N HCl (10 mL), water (2×10 mL), and saturated NaCl (2×10 mL). Dried over MgSO4 and filtered. The solvent was removed under reduced pressure and the product was purified by column chromatography (EtOAc/hexanes 1:1) to afford 54 as a pale yellow solid (117 mg, 60%); MS m/z: 434 (M+H)+. Anal. Calcd. For, C19H19N3O3S2: C, 52.63; H, 4.42; N, 9.69; S, 22.19. Found: C, 52.69; H, 4.49; N, 9.54; S, 22.11.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08916550B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-df825a03d2754247ad26d89b135b6ddb |
| Source note | uspto-grants-2014_12 |