HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,4,6-Trimethylpyridine → HCID 54270920, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,4,6-Trimethylpyridine | HCID 7953 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | HCID 53695575 | HCID 53695575 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 54270920 | HCID 54270920 | 38.4% |
Reaction Steps
A solution of Example 3C (0.85 g, 3.24 mmol), collidine (0.94 mL, 7.13 mmol) and lithium chloride (0.21 g, 4.97 mmol) in DMF (10 mL) at 0° C. was treated with methanesulfonyl chloride (0.38 mL, 4.87 mmol), stirred 16 hours at room temperature, poured into aqueous ammonium chloride, and extracted with ethyl acetate. The ethyl acetate was washed with water, brine, dried (MgSO4), filtered, concentrated, and purified on silica gel with 3% ethyl acetate/hexanes to provide 0.35 g (38%) of the desired compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06288261B1 |
| Source dataset | uspto-grants-2001_09 |
| ORD ID | ord-f86d65187ebf49978179d63f9dadab84 |
| Source note | uspto-grants-2001_09 |